Thiophosgene → HCID 82491428、化合物

HRID 1398893ノート

反応式

HRID 1398893 の反応式
[Cl:1][C:2]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][C:3]=1[NH2:4].[C:11](Cl)(Cl)=[S:12]>C(=O)([O-])O.[Na+].O1CCCC1>[Cl:1][C:2]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][C:3]=1[N:4]=[C:11]=[S:12]

参加物

5

反応物 2

HCID 10040ThiophosgeneHCID 4074322-Chloro-4-methoxyaniline

生成物 1

HCID 82491428HCID 82491428、化合物収率 68.5%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 516892Sodium Bicarbonate溶媒

実験手順

To a stirred solution of 2-chloro-4-methoxyaniline (7.90 g, 50.1 mmol) in saturated aqueous sodium hydrogen carbonate (40 mL) and tetrahydrofuran (40 mL) was added thiophosgene (4.99 mL, 65.1 mmol) at room temperature. After 30 min, the reaction mixture was extracted with ethyl acetate, washed with aqueous sodium hydrogen carbonate and brine, dried over sodium sulfate, filtrated, and concentrated in vacuo. The resulting solid was washed with n-hexane to give the title compound as a pale red solid (6.85 g, 34.3 mmol, 68%).

後処理

  1. extractionthe reaction mixture was extracted with ethyl acetate
  2. washwashed with aqueous sodium hydrogen carbonate and brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltrated
  5. concentrationconcentrated in vacuo
  6. washThe resulting solid was washed with n-hexane

出典と根拠

ORDレコード
ord-1825ea416a7c4713a2dfce147b439e65
出典データセット
uspto-grants-2014_12
特許番号
US08901141B2

反応ノート

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