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Triethylamine → HCID 20144930, 화합물

HRID 648498
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HRID 648498 반응식
Cl.[F:2][C:3]([F:25])([F:24])[C:4]1[CH:13]=[C:12]2[C:7]([C:8]([NH:14][C:15]3[CH:23]=[CH:22][C:18]([C:19]([Cl:21])=[O:20])=[CH:17][CH:16]=3)=[CH:9][CH:10]=[N:11]2)=[CH:6][CH:5]=1.Cl.[F:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[S:34]([CH:37]1[CH2:42][CH2:41][NH:40][CH2:39][CH2:38]1)(=[O:36])=[O:35].C(N(CC)CC)C>C(Cl)Cl>[ClH:21].[F:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[S:34]([CH:37]1[CH2:42][CH2:41][N:40]([C:19](=[O:20])[C:18]2[CH:22]=[CH:23][C:15]([NH:14][C:8]3[C:7]4[C:12](=[CH:13][C:4]([C:3]([F:25])([F:24])[F:2])=[CH:5][CH:6]=4)[N:11]=[CH:10][CH:9]=3)=[CH:16][CH:17]=2)[CH2:39][CH2:38]1)(=[O:35])=[O:36]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 13603946HCID 13603946, 화합물HCID 13825033HCID 13825033, 화합물

생성물 1

HCID 20144930HCID 20144930, 화합물수율 46.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

(B 5) 4-[[7-(Trifluoromethyl)-4-quinolyl]amino]benzoyl chloride hydrochloride (65.20 g) was added slowly to a stirred mixture of 4-[(2-fluorophenyl)sulfonyl]piperidine hydrochloride (47.0 g) and triethylamine (117.2 ml) in dry methylene chloride (1.01 l) at room temperature. The resultant mixture was stirred at the same temperature for 1 hour and under ice cooling for 0.5 hours. The precipitated powder was collected by filtration, washed with a mixture of methylene chloride and water, and suspended in a mixture of chloroform and methanol. Excess methanolic hydrochloric acid was added to the suspension and the resulting solution was concentrated in vacuo to give an oil. The oil was triturated in a mixture of ethyl acetate and ethanol to give powdery 4-[(2-fluorophenyl)sulfonyl]-1-[4-[[7-(trifluoromethyl)-4-quinolyl]amino]benzoyl]piperidine hydrochloride (46.73 g).

후처리

  1. filtrationThe precipitated powder was collected by filtration
  2. washwashed with a mixture of methylene chloride and water
  3. additionsuspended in a mixture of chloroform and methanol
  4. additionExcess methanolic hydrochloric acid was added to the suspension
  5. concentrationthe resulting solution was concentrated in vacuo
  6. customto give an oil
  7. customThe oil was triturated in a mixture of ethyl acetate and ethanol

출처 및 근거

ORD 기록
ord-68169c71ecec4d48bc306bf092c37756
출처 데이터셋
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04735952

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