Thiophosgene → 3-Chloro-4-isothiocyanato-benzonitrile

HRID 2407517ノート

反応式

HRID 2407517 の反応式
[C:1](Cl)(Cl)=[S:2].[NH2:5][C:6]1[CH:13]=[CH:12][C:9]([C:10]#[N:11])=[CH:8][C:7]=1[Cl:14]>O>[Cl:14][C:7]1[CH:8]=[C:9]([CH:12]=[CH:13][C:6]=1[N:5]=[C:1]=[S:2])[C:10]#[N:11]

参加物

4

反応物 2

HCID 10040ThiophosgeneHCID 5198964-Amino-3-chlorobenzonitrile

生成物 1

HCID 183163923-Chloro-4-isothiocyanato-benzonitrile

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a suspension of thiophosgene (2 mL) in water (5 mL) was added 4-amino-3-chloro-benzonitrile (1 g, 7 mmol) in small portions over a period of 1 h at 25° C. The mixture was extracted with ethyl acetate (3×25 mL). Combined organic phase was washed with brine (1×50 mL), dried (MgSO4) and concentrated to dryness in vacuo. The title compound 3d was obtained as a tan solid (1.3 g, 96% yield).

後処理

  1. extractionThe mixture was extracted with ethyl acetate (3×25 mL)
  2. washCombined organic phase was washed with brine (1×50 mL)
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated to dryness in vacuo

出典と根拠

ORDレコード
ord-90fc7827956e45d5861cd869e18723af
出典データセット
uspto-grants-2014_08
特許番号
US08809550B2

反応ノート

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