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4-Chlorophenyl isothiocyanate → tert-Butyl 4-{[(4-chlorophenyl)amino]carbonothioyl}-1,4-diazepane-1-carboxylate

HRID 20278
ノート
印刷プレビュー

反応式

HRID 20278 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]=[S:10])=[CH:4][CH:3]=1.[C:11]([N:18]1[CH2:24][CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1)([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12]>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([N:21]2[CH2:22][CH2:23][CH2:24][N:18]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:19][CH2:20]2)=[S:10])=[CH:4][CH:3]=1
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 2

HCID 164804-Chlorophenyl isothiocyanateHCID 2756058Tert-butyl 1,4-diazepane-1-carboxylate

生成物 1

HCID 59347509tert-Butyl 4-{[(4-chlorophenyl)amino]carbonothioyl}-1,4-diazepane-1-carboxylate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 4-chlorophenyl isothiocyanate (5.0 g, 29.95 mmol), and BOC-homopiperazine (6.0 g, 29.95 mmol) in ethanol (50 mL) was stirred at room temperature for 2 hours. The mixture was evaporated under reduced pressure, the residue was partitioned between ethyl acetate and water and the layers were separated. The organic phase was dried over MgSO4 and evaporated under reduced pressure to give the title compound as a white foam.

後処理

  1. customThe mixture was evaporated under reduced pressure
  2. customthe residue was partitioned between ethyl acetate and water
  3. customthe layers were separated
  4. dry with materialThe organic phase was dried over MgSO4
  5. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-daa6eab60c9e4f4fa2b20aee2c27aaac
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07745630B2

反応ノート

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