Sodium Bicarbonate → HCID 68638439, 화합물

HRID 2196453노트

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HRID 2196453 반응식
Br[CH:2]([CH3:10])[C:3]([C:5]1[S:6][CH:7]=[CH:8][CH:9]=1)=O.C(=O)([O-])O.[Na+].[Si:16]([O:23][CH2:24][C:25]1[CH:26]=[C:27]([C:31]2[CH:32]=[CH:33][C:34]([NH2:37])=[N:35][CH:36]=2)[CH:28]=[CH:29][CH:30]=1)([C:19]([CH3:22])([CH3:21])[CH3:20])([CH3:18])[CH3:17]>C(O)C>[Si:16]([O:23][CH2:24][C:25]1[CH:26]=[C:27]([C:31]2[CH:32]=[CH:33][C:34]3[N:35]([C:2]([CH3:10])=[C:3]([C:5]4[S:6][CH:7]=[CH:8][CH:9]=4)[N:37]=3)[CH:36]=2)[CH:28]=[CH:29][CH:30]=1)([C:19]([CH3:22])([CH3:21])[CH3:20])([CH3:18])[CH3:17]

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 117699522-Bromo-1-(thiophen-2-yl)propan-1-oneHCID 442323785-[3-(tert-Butyldimethylsilanyloxymethyl)phenyl]pyridin-2-ylamine

생성물 1

HCID 68638439HCID 68638439, 화합물수율 67.2%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
100 °C

실험 절차

In a glass tube, 280 mg of 5-[3-(tert-butyldimethylsilanyloxymethyl)phenyl]pyridin-2-ylamine, 390 mg of 2-bromo-1-thiophen-2-ylpropan-1-one and 190 mg of sodium hydrogencarbonate are dissolved in 5 ml of ethanol. The tube is closed and heated at 100° C. for 20 h. After cooling, the mixture is concentrated under reduced pressure. The residue is purified by silica gel chromatography, elution being carried out with a heptane/ethyl acetate mixture. 260 mg of compound are obtained.

후처리

  1. customThe tube is closed
  2. temperatureAfter cooling
  3. concentrationthe mixture is concentrated under reduced pressure
  4. customThe residue is purified by silica gel chromatography, elution

출처 및 근거

ORD 기록
ord-74952a896aff4453826db99d96a0be16
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08338451B2

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