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Dichloromethane → 3-(3-[(2-Chloro-3-trifluoromethyl-benzyl)-diphenylethyl-amino]-propoxy}-phenylamine dihydrochloride

HRID 902639
ノート
印刷プレビュー

反応式

HRID 902639 の反応式
C(OC(=O)[NH:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][CH2:15][CH2:16][CH2:17][N:18]([CH2:33][C:34]2[CH:39]=[CH:38][CH:37]=[C:36]([C:40]([F:43])([F:42])[F:41])[C:35]=2[Cl:44])[CH2:19][CH:20]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH:9]=1)(C)(C)C.C(Cl)[Cl:47].FC(F)(F)C(O)=O>CCOCC.Cl>[ClH:44].[ClH:47].[Cl:44][C:35]1[C:36]([C:40]([F:41])([F:42])[F:43])=[CH:37][CH:38]=[CH:39][C:34]=1[CH2:33][N:18]([CH2:19][CH:20]([C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1)[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[CH2:17][CH2:16][CH2:15][O:14][C:10]1[CH:9]=[C:8]([NH2:7])[CH:13]=[CH:12][CH:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 10175511(3-{3-[(2-Chloro-3-trifluoromethyl-benzyl)-diphenylethyl-amino]-propoxy}-phenyl)-carbamic acid tert-butyl ester

生成物 1

HCID 865982843-(3-[(2-Chloro-3-trifluoromethyl-benzyl)-diphenylethyl-amino]-propoxy}-phenylamine dihydrochloride

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid
溶媒
HCID 3283Diethyl Ether溶媒2 回

実験手順

(3-{3-[(2-Chloro-3-trifluoromethyl-benzyl)-diphenylethyl-amino]-propoxy}-phenyl)-carbamic acid tert-butyl ester, (0.51 g, 0.8 mmol) was stirred overnight at room temperature in a mixture methylene chloride (5 mL) and trifluoroacetic acid (0.5 mL). The solvents were removed in vacuo to yield the crude amine as an oil. The oil was diluted with ether, and 1 N HCl in Et2O was added to precipitate the HCl salt of the product. The title compound was isolated as a cream yellow powder, 0.53 g (100%). MS (ESI) 539 (M+H+).

後処理

  1. customThe solvents were removed in vacuo
  2. customto yield the crude amine as an oil
  3. additionwas added
  4. customto precipitate the HCl salt of the product

出典と根拠

ORDレコード
ord-8d499415fe4d4ba39c0345b9e1d9912a
出典データセット
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07365085B2

反応ノート

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