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CAS RN: 148893-10-1 | 产品编码: R0295
Reagents for Condensation Reactions (HATU) (HPMC encapsulated)
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Contents (per one capsule)
- HATU : ca. 0.45 mmol
Directions for Use
- Each capsule contains all reagents for a single use on 0.40 mmol scale condensation reaction (amide coupling reaction) between carboxylic acid and amine.
Typical condition: 0.40 mmol of carboxylic acid and 1.05 equiv. of amines and 1.5 equiv. of base in DMF (0.20 M) at 30 °C.
Related Products
- A1797 HATU
| 产品编码 | R0295 |
| 分子式/分子量 | C__1__0H__1__5F__6N__6OP = 380.24 |
| 外观与形状（20°C） | 固体 |
| 储存温度 | 冷藏 (0-10°C) |
| 应避免的情况 | 加热 |
| CAS RN | 148893-10-1 |
技术规格
| Appearance | White to Almost white capsule |
| Functionality test (conversion ratio) | min. 95.0 % |
物性（参考值）
GHS
| 象形图 |
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| 信号词 | Danger |
| 危险性说明 | H317 : May cause an allergic skin reaction. H334 : May cause allergy or asthma symptoms or breathing difficulties if inhaled. |
| 防范说明 | P501 : Dispose of contents/ container to an approved waste disposal plant. P261 : Avoid breathing dust. P272 : Contaminated work clothing should not be allowed out of the workplace. P280 : Wear protective gloves. P284 : Wear respiratory protection. P302 + P352 : IF ON SKIN: Wash with plenty of water. P342 + P311 : If experiencing respiratory symptoms: Call a POISON CENTER/doctor. P362 + P364 : Take off contaminated clothing and wash it before reuse. P304 + P340 : IF INHALED: Remove person to fresh air and keep comfortable for breathing. P333 + P313 : If skin irritation or rash occurs: Get medical advice/ attention. |
相关法规
运输信息
| HS编码* | 3822.19-000 |
应用
TCI Practical Example: The Condensation Reaction Using HATU in a Capsule Reagent
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Used Chemicals
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Procedure
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Reagents for condensation capsule (HATU) (one capsule) was added to a solution of 4-bromobenzoic acid (80 mg, 0.40 mmol, 1.0 eq.), morpholine (37 μL, 0.42 mmol, 1.05 eq.) and N,N-diisopropylethylamine (100 μL, 0.60mmol, 1.5 eq.) in DMF (2 mL) at r.t. and the mixture was stirred at 30 °C for 1 hour. The reaction solution was diluted with sat. Na2SO4 aq. (15 mL) and extracted with ethyl acetate (15 mL x 2). The organic layer was washed with 2 mol/L HCl aq. (15 mL), sat. NaHCO3 aq. (15 mL) and brine (15 mL), dried over anhydrous sodium sulfate and concentrated under reduced pressure. The crude product was purified by silica gel chromatography (hexane:ethylacetate = 2:1 - 1:1) to afford (4-bromophenyl)(morpholino)methanone (95 mg, 88% yield) as a white solid.
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Experimenter’s Comments
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The reaction mixture was monitored by UPLC.
The shape of the capsule is like below image and each capsule includes HATU (ca. 0.40 mmol).
The material of the capsule is water-soluble HPMC (hydroxypropyl methylcellulose).
HPMC was removed with a saturated sodium sulfate solution, but during the separation, the separating funnel was clogged due to the precipitation of sodium sulfate. Therefore, the precipitated sodium sulfate was filtered off, and ethyl acetate was added to the filtrate for extraction. Use of a more dilute sodium sulfate solution may reduce clogging problems.
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Analytical Data
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(4-Bromophenyl)(morpholino)methanone
1H NMR (400 MHz, CDCl3); δ 7.57 (d, J = 8.4 Hz, 2H), 7.30 (d, J = 8.4 Hz, 2H), 3.74-3.44 (m, 8H).
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Lead Reference
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- Hydrophobic Pockets of HPMC Enable Extremely Short Reaction Times in Water
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Other Reference
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- HPMC: A Biomass-Based Semisynthetic Sustainable Additive Enabling Clean and Fast Chemistry in Water
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