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

HRID 586057ノート

反応式

HRID 586057 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 131183231-Chloro-4-(2-isocyanatopropan-2-yl)benzene

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c6ece5df910d4d219340451d97ad35f1
出典データセット
uspto-grants-2005_08
特許番号
US06933311B2

反応ノート

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