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

HRID 586057노트

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HRID 586057 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)benzene

시약·촉매·용매 1

HCID 962Water용매

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온도
0 °C

실험 절차

The product from Example 297A (4.00 g, 19.4 mmol) in acetone (9 mL) at 0° C. ws treated with 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 toluene solution was dried over MgSO4, filtered, and the filtrate was heated to reflux for 1 hour. The cooled solution was concentrated under reduced pressure to provide the title compound.

후처리

  1. extractionthe mixture was extracted with toluene (20 mL)
  2. dry with materialThe toluene solution was dried over MgSO4
  3. filtrationfiltered
  4. temperaturethe filtrate was heated
  5. temperatureto reflux for 1 hour
  6. concentrationThe cooled solution was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-c6ece5df910d4d219340451d97ad35f1
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06933311B2

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