2-Chlorobenzylamine → 1-Chloro-2-(isocyanatomethyl)benzene

HRID 650102

反応式

HRID 650102 の反応式
[Cl:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4][NH2:5].Cl[C:11](Cl)([O:13]C(=O)OC(Cl)(Cl)Cl)Cl.C([O-])(O)=O.[Na+]>C(Cl)Cl.O>[Cl:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4][N:5]=[C:11]=[O:13]

参加物

6

反応物 3

HCID 666482-ChlorobenzylamineHCID 94429TriphosgeneHCID 516892Sodium Bicarbonate

生成物 1

HCID 27333671-Chloro-2-(isocyanatomethyl)benzene収率 232.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-chlorobenzylamine (1.0 g, 7.06 mmol) in a mixture of CH2Cl2 and H2O (10 mL/10 mL), triphosgene (838 mg, 2.82 mmol) and NaHCO3 (1.78 g, 21.2 mmol) were added. The reaction mixture was stirred at room temperature for 16 hours. Then the reaction mixture was partitioned between CH2Cl2 and water. The combined organic layers are dried over MgSO4 and filtered. The solvent was evaporated to give the desired product (1.1 g, 93%). EI-MS m/z 168.7 (M+).

後処理

  1. additionwere added
  2. customThen the reaction mixture was partitioned between CH2Cl2 and water
  3. dry with materialThe combined organic layers are dried over MgSO4
  4. filtrationfiltered
  5. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-291c8d96be1d44cfb70e9e6690479ef3
出典データセット
uspto-grants-2001_08
特許番号
US06271261B1

関連ノート

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