Thiophosgene → HCID 82491428, 화합물

HRID 1628536노트

반응식

HRID 1628536 반응식
[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]

참가 물질

5

반응물 2

HCID 10040ThiophosgeneHCID 4074322-Chloro-4-methoxyaniline

생성물 1

HCID 82491428HCID 82491428, 화합물수율 68.5%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 516892Sodium Bicarbonate용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-65fb0c54d72945e4b364a45769af1cac
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785460B2

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