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(3,4-Difluoro-benzyl)-(3-methyl-benzo[b]thiophen-2-yl)-carbamic acid tert-butyl ester → (3,4-Difluoro-benzyl)-(3-methyl-benzo[b]thiophen-2-yl)-amine

HRID 1691546
ノート
印刷プレビュー

反応式

HRID 1691546 の反応式
C(OC(=O)[N:7]([CH2:18][C:19]1[CH:24]=[CH:23][C:22]([F:25])=[C:21]([F:26])[CH:20]=1)[C:8]1[S:12][C:11]2[CH:13]=[CH:14][CH:15]=[CH:16][C:10]=2[C:9]=1[CH3:17])(C)(C)C>ClCCl.FC(F)(F)C(O)=O>[F:26][C:21]1[CH:20]=[C:19]([CH:24]=[CH:23][C:22]=1[F:25])[CH2:18][NH:7][C:8]1[S:12][C:11]2[CH:13]=[CH:14][CH:15]=[CH:16][C:10]=2[C:9]=1[CH3:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 57920462(3,4-Difluoro-benzyl)-(3-methyl-benzo[b]thiophen-2-yl)-carbamic acid tert-butyl ester

生成物 1

HCID 57920455(3,4-Difluoro-benzyl)-(3-methyl-benzo[b]thiophen-2-yl)-amine

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

A solution of compound 125-C (2.7 g, 6.9 mmol) in dichloromethane (40 mL) and trifluoroacetic acid (40 mL) was stirred at rt for 4 h. The solvent was evaporated in vacuo, and the residue partitioned between dichloromethane and saturated aqueous sodium bicarbonate. The organic layer was dried over sodium sulfate, and the solvent evaporated in vacuo to afford compound 125-D as a colorless solid (1.86 g, 93%). 1H-NMR (CDCl3): δ 2.16 (s, 3H), 4.37 (s, 2H), 7.09-7.32 (m, 5H), 7.40 (d, 1H), 7.60 (d, 1H); MS: m/z 290.1 (MH+).

後処理

  1. customThe solvent was evaporated in vacuo
  2. customthe residue partitioned between dichloromethane and saturated aqueous sodium bicarbonate
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. customthe solvent evaporated in vacuo
  5. customto afford compound 125-D as a colorless solid (1.86 g, 93%)

出典と根拠

ORDレコード
ord-97ea309fd5124e5b9f45915ea87a92eb
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08153682B2

反応ノート

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