Dichloromethane → HCID 69351600, 화합물

HRID 1005659노트

반응식

HRID 1005659 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:15]=[CH:16][CH:17]=[C:18]3[C:22]=2[NH:21][CH:20]=[C:19]3[S:23]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)(=[O:25])=[O:24])[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O.[Cl:39]CCl>>[ClH:39].[C:26]1([S:23]([C:19]2[C:18]3[C:22](=[C:14]([N:11]4[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]4)[CH:15]=[CH:16][CH:17]=3)[NH:21][CH:20]=2)(=[O:24])=[O:25])[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1

참가 물질

4

반응물 3

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 60108791HCID 60108791, 화합물

생성물 1

HCID 69351600HCID 69351600, 화합물

실험 절차

4-(3-Benzenesulfonyl-1H-indol-7-yl)-piperazine-1-carboxylic acid tert-butyl ester (1 g, 2.2 mmol) was dissolved in 5 mL of dichloromethane and 6 mL of trifluoroacetic acid was added. After 10 min the mixture was concentrated in vacuo, taken into water, and washed with ether. The aqueous layer was basified with ammonium hydroxide, extracted with dichloromethane, and the extract was dried (sodium sulfate) and evaporated to afford the crude free base. The hydrochloride salt was crystallized from ethanol to afford 550 mg of 3-benzenesulfonyl-7-piperazin-1-yl-1H-indole hydrochloride (101), m.p. 278-280° C.

후처리

  1. concentrationAfter 10 min the mixture was concentrated in vacuo
  2. washwashed with ether
  3. extractionextracted with dichloromethane
  4. dry with materialthe extract was dried (sodium sulfate)
  5. customevaporated
  6. customto afford the crude free base
  7. customThe hydrochloride salt was crystallized from ethanol

출처 및 근거

ORD 기록
ord-5950f714b95e44fa824208c5b0834406
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06787535B2

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