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Triethylamine → HCID 68643979, 화합물

HRID 2388702
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HRID 2388702 반응식
[C:1]1([CH:7]2[CH:12]=[C:11]([N:13]3[CH2:17][CH2:16][CH2:15][CH2:14]3)[CH2:10][CH2:9][N:8]2[C:18](=[O:20])[CH3:19])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[C:22](=[N:28][OH:29])[C:23]([O:25][CH2:26][CH3:27])=[O:24].C(N(CC)CC)C>ClCCl>[C:18]([N:8]1[CH2:9][CH2:10][C:11]2([N:13]3[CH2:14][CH2:15][CH2:16][CH2:17]3)[O:29][N:28]=[C:22]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:12]2[CH:7]1[C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)(=[O:20])[CH3:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 6816376Ethyl chloro(hydroximino)acetateHCID 68643976HCID 68643976, 화합물

생성물 1

HCID 68643979HCID 68643979, 화합물수율 80%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 1-(2-phenyl-4-(pyrrolidin-1-yl)-5,6-dihydropyridin-1(2H)-yl)ethanone in dichloromethane (15 mL) was added a solution of ethyl 2-chloro-2-(hydroxyimino)acetate (4.709 mmol, 1.4 eq.) in dichloromethane (5 ml) at 0° C. Then triethylamine (1.4 eq.) was added dropwise at same reaction conditions and the mixture was stirred at room temperature overnight. The reaction mixture was quenched with 10% citric acid solution and extracted with dichloromethane (3×). The combined organic layers were washed with saturated sodium bicarbonate solution and brine, dried over sodium sulfate, concentrated to dryness to give the desired product, which was used in the next step without further purification.

후처리

  1. customThe reaction mixture was quenched with 10% citric acid solution
  2. extractionextracted with dichloromethane (3×)
  3. washThe combined organic layers were washed with saturated sodium bicarbonate solution and brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-7cb4966bdba4478da42e06ca95fd7622
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08268814B2

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