Dichloromethane → HCID 69351600、化合物

HRID 1005659ノート

反応式

HRID 1005659 の反応式
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

参加物

4

反応物 3

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 60108791HCID 60108791、化合物

生成物 1

HCID 69351600HCID 69351600、化合物

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5950f714b95e44fa824208c5b0834406
出典データセット
uspto-grants-2004_09
特許番号
US06787535B2

反応ノート

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