Hydrochloric Acid → HCID 69253147、化合物

HRID 902701ノート

反応式

HRID 902701 の反応式
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

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 69252373HCID 69252373、化合物

生成物 1

HCID 69253147HCID 69253147、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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+).

後処理

  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)

出典と根拠

ORDレコード
ord-3d602e8c7c4f475982d52a4b380b2533
出典データセット
uspto-grants-2008_04
特許番号
US07365085B2

反応ノート

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