Acetone → 1-Chloro-4-(2-isocyanatopropan-2-yl)benzene

HRID 585941노트

반응식

HRID 585941 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([CH3:13])([CH3:12])C(Cl)=O)=[CH:4][CH:3]=1.[N-:14]=[N+]=[N-].[Na+].C[C:19](C)=[O:20]>O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([N:14]=[C:19]=[O:20])([CH3:12])[CH3:13])=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 180AcetoneHCID 33557Sodium AzideHCID 135368632-(4-Chlorophenyl)-2-methylpropanoyl chloride

생성물 1

HCID 131183231-Chloro-4-(2-isocyanatopropan-2-yl)benzene수율 96%

시약·촉매·용매 1

HCID 962Water용매

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온도
0 °C

실험 절차

The product of Example 76A (4.00 g, 19.4 mmol) in acetone (9 mL) at 0° C. was treated with a solution of sodium azide (1.27 g) in water (9 mL) dropwise over 15 minutes. After stirring for 30 minutes at 0° C., the mixture was extracted with toluene (20 mL). The organic extract was dried with MgSO4, filtered, and the filtrate heated at reflux for 1 hour. The mixture was allowed to cool to room temperature and was concentrated under reduced pressure to provide the title compound as a pale yellow oil (3.45 g, 96%).

후처리

  1. extractionthe mixture was extracted with toluene (20 mL)
  2. extractionThe organic extract
  3. dry with materialwas dried with MgSO4
  4. filtrationfiltered
  5. temperaturethe filtrate heated
  6. temperatureat reflux for 1 hour
  7. temperatureto cool to room temperature
  8. concentrationwas concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-293dbff1e4eb40c49e1a5610106bb9f1
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06933311B2

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