Methyl Isocyanate → N-Methyl-N(4-t-Butylphenylthiosulfenyl) Carbamoyl Fluoride

HRID 838917ノート

反応式

HRID 838917 の反応式
[FH:1].[CH3:2][N:3]=[C:4]=[O:5].[C:6]([C:10]1[CH:15]=[CH:14][C:13]([S:16][S:17]Cl)=[CH:12][CH:11]=1)([CH3:9])([CH3:8])[CH3:7]>C1(C)C=CC=CC=1>[CH3:2][N:3]([S:17][S:16][C:13]1[CH:14]=[CH:15][C:10]([C:6]([CH3:9])([CH3:8])[CH3:7])=[CH:11][CH:12]=1)[C:4]([F:1])=[O:5]

参加物

5

反応物 3

HCID 12228Methyl IsocyanateHCID 14917Hydrofluoric AcidHCID 205604854-t-Butylphenylthiosulfenyl chloride

生成物 1

HCID 23333006N-Methyl-N(4-t-Butylphenylthiosulfenyl) Carbamoyl Fluoride

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a solution of 5.5 g hydrogen fluoride in toluene cooled to -65° C was added dropwise with stirring 15.0 ml of methylisocyanate over a period of 20 minutes after stirring for 1.5 hr preshly prepared 4-t-butylphenylthiosulfenyl chloride (prepared from 36.2 g 4-butylphenol and 31.0 g sulfur dichloride in 800 ml ethyl ether) was added at -10° to 0° C over a period of 0.5 hr. After stirring overnight at ambient temperature, the salt was removed by filtration and the filtrate distilled. b.p. 122°-127° C/0.2 Torr.

後処理

  1. additionwas added dropwise
  2. additionwas added at -10° to 0° C over a period of 0.5 hr
  3. customthe salt was removed by filtration
  4. distillationthe filtrate distilled

出典と根拠

ORDレコード
ord-529877a0ccb54820af61aecc2cca9f4f
出典データセット
uspto-grants-1978_06
特許番号
US04093652

反応ノート

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