Hydrochloric Acid → HCID 69253147, 화합물

HRID 902701노트

반응식

HRID 902701 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([O:20][CH2:21][CH2:22][CH2:23][N:24]([CH2:39][C:40]3[CH:45]=[CH:44][CH:43]=[C:42]([C:46]([F:49])([F:48])[F:47])[C:41]=3[Cl:50])[CH2:25][CH:26]([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)[C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[CH:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.Cl>CO>[ClH:50].[Cl:50][C:41]1[C:42]([C:46]([F:48])([F:47])[F:49])=[CH:43][CH:44]=[CH:45][C:40]=1[CH2:39][N:24]([CH2:25][CH:26]([C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1)[C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)[CH2:23][CH2:22][CH2:21][O:20][C:16]1[CH:17]=[CH:18][CH:19]=[C:14]([N:11]2[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)[CH:15]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 69252373HCID 69252373, 화합물

생성물 1

HCID 69253147HCID 69253147, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 4-(3-{3-[(2-chloro-3-trifluoromethyl-benzyl)-diphenylethyl-amino]-propoxy}-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (475 mg, 0.67 mmol) in a 1:1 mixture of 3M HCl (aq.) and methanol (30 mL total) was stirred at room temperature for 18 hours. The mixture was concentrated in vacuo, and the crude material was dissolved in EtOAc. The EtOAc solution was washed with saturated aqueous sodium bicarbonate solution (3×) and brine (1×), dried over sodium sulfate, and filtered. The EtOAc extracts were concentrated and the crude piperazine was treated with 1 M HCl (Et2O) to afford the title compound as a solid, 415 mg (100%). MS(ES) m/e 608.4 (M+).

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. dissolutionthe crude material was dissolved in EtOAc
  3. washThe EtOAc solution was washed with saturated aqueous sodium bicarbonate solution (3×) and brine (1×)
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationThe EtOAc extracts were concentrated
  7. additionthe crude piperazine was treated with 1 M HCl (Et2O)

출처 및 근거

ORD 기록
ord-3d602e8c7c4f475982d52a4b380b2533
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07365085B2

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