1,1,1,3,3,3-Hexafluoro-2-propanol → Hexafluoroisopropyl beta-chloroisobutyrylcarbamate

HRID 1707517ノート

反応式

HRID 1707517 の反応式
[Cl:1][CH2:2][CH:3]([CH3:9])[C:4]([N:6]=[C:7]=[O:8])=[O:5].[CH:10]([OH:19])([C:15]([F:18])([F:17])[F:16])[C:11]([F:14])([F:13])[F:12]>C(Cl)(Cl)Cl>[Cl:1][CH2:2][CH:3]([CH3:9])[C:4]([NH:6][C:7](=[O:8])[O:19][CH:10]([C:15]([F:18])([F:17])[F:16])[C:11]([F:14])([F:13])[F:12])=[O:5]

参加物

4

反応物 2

HCID 135291,1,1,3,3,3-Hexafluoro-2-propanolHCID 137662253-Chloro-2-methylpropanoyl isocyanate

生成物 1

HCID 53764557Hexafluoroisopropyl beta-chloroisobutyrylcarbamate

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a solution of beta-chloroisobutyryl isocyanate (7.38 g; 50 mmol) in chloroform (50 ml), a solution of 1,1,1,3,3,3-hexafluoroisopropanol (8.4 g; 50 mmol) in chloroform (10 ml) was dropwise added at 10° C. under ice-cooling. After completion of the addition, the resultant mixture was stirred for 1 hour, whereby hexafluoroisopropyl beta-chloroisobutyrylcarbamate was produced. A solution of triethylamine (5.05 g; 50 mmol) in chloroform (50 ml) was added to the reaction mixture in 30 minutes under ice-cooling. The reaction mixture was stirred for 1 hour, and precipitated triethylamine hydrochloride (6.87 g) was eliminated by filtration. The filtrate was concentrated under reduced pressure to give hexafluoroisopropyl N-methacryloylcarbamate (13.4 g), which was recrystallized from benzene to give colorless prisms. M.P., 112.5°-113° C.

後処理

  1. temperaturecooling
  2. additionAfter completion of the addition

出典と根拠

ORDレコード
ord-77a2cb1b87554a1997117baafbd43afc
出典データセット
uspto-grants-1994_10
特許番号
US05354495

反応ノート

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