Chloroform → HCID 69960173, 화합물

HRID 893849

반응식

HRID 893849 반응식
C(Cl)(Cl)Cl.[CH2:5]([O:7][C:8]([CH:10]1[CH:18]2[C:13]3([CH:22]=[CH:21][CH:20]=[CH:19][C:14]3=[N:15][CH2:16][CH2:17]2)[S:12][CH2:11]1)=[O:9])[CH3:6].[Cl:23][C:24]1[CH:32]=[CH:31][CH:30]=[CH:29][C:25]=1[C:26](Cl)=[O:27]>C(N(CC)CC)C>[CH2:5]([O:7][C:8]([CH:10]1[CH:18]2[C:13]3([CH:22]=[CH:21][CH:20]=[CH:19][C:14]3=[N:15][CH2:16][CH2:17]2)[S:12][CH:11]1[C:26](=[O:27])[C:25]1[CH:29]=[CH:30][CH:31]=[CH:32][C:24]=1[Cl:23])=[O:9])[CH3:6]

참가 물질

5

반응물 3

HCID 6212ChloroformHCID 691102-Chlorobenzoyl chlorideHCID 199609281,2,3,4-Tetrahydro-benzo[b]thieno[2,3,c]pyridine-3-carboxylic acid ethyl ester

생성물 1

HCID 69960173HCID 69960173, 화합물수율 67.1%

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

To 30 ml of chloroform were added 0.60 g of 1,2,3,4-tetrahydro-benzo[b]thieno[2,3-c]pyridine-3-carboxylic acid ethyl ester synthesized in Example 1, 0.64 ml of triethylamine, and 523 mg of 2-chlorobenzoyl chloride, and the mixture was stirred for one hour at room temperature. The reaction mixture was washed with ml of water and then with 30 ml of an aqueous sodium hydrogencarbonate solution having a pH of 9.0, and also with 30 ml of water. The chloroform layer was dried by sodium sulfate and the solvent was distilled off under reduced pressure to provide 614 mg (yield of 67%) of 2 -(2-chlorobenzoyl)-1,2,3,4-tetrahydro-benzo[b]thieno[2,3-c]pyridine-3-carboxylic acid ethyl ester.

후처리

  1. washThe reaction mixture was washed with ml of water
  2. dry with materialThe chloroform layer was dried by sodium sulfate
  3. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-2b6f45eeb7b846339153ff74b09d8d97
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05126448

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