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Diethyl Ether → O-[3-(2,2-Dimethoxyethylthio)phenyl] N-Methylcarbamate

HRID 972116
ノート
印刷プレビュー

反応式

HRID 972116 の反応式
[CH3:1][O:2][CH:3]([O:13][CH3:14])[CH2:4][S:5][C:6]1[CH:7]=[C:8]([OH:12])[CH:9]=[CH:10][CH:11]=1.[CH3:15][N:16]=[C:17]=[O:18].CCOCC>C1C=CC=CC=1.CN(C)C>[CH3:15][NH:16][C:17](=[O:18])[O:12][C:8]1[CH:9]=[CH:10][CH:11]=[C:6]([S:5][CH2:4][CH:3]([O:2][CH3:1])[O:13][CH3:14])[CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 3283Diethyl EtherHCID 12228Methyl Isocyanate2 回HCID 203966733-(2,2-Dimethoxyethylthio)phenol

生成物 1

HCID 20396660O-[3-(2,2-Dimethoxyethylthio)phenyl] N-Methylcarbamate

試薬・触媒・溶媒 2

HCID 1146Trimethylamine触媒HCID 241Benzene溶媒2 回

実験手順

3-(2,2-Dimethoxyethylthio)phenol (1.80 grams) dissolved in benzene (5 ml) was charged into a glass reaction vessel equipped with a mechanical stirrer. Methyl isocyanate (12 ml) and trimethylamine (2 drops) were then added, and the resulting mixture was stirred at room temperature for a period of about 51/2 hours. The mixture was then allowed to stand overnight and was then stripped of excess methyl isocyanate and a portion of the benzene. The concentrated solution was then added to ether and cooled to -60° C., resulting in a precipitate. The precipitate was recrystallized from ether to yield the desired product O-[3-(2,2-dimethoxyethylthio)phenyl]-0 N-methylcarbamate having a melt point of 46° to 48° C.

後処理

  1. additionwas charged into a glass reaction vessel
  2. customequipped with a mechanical stirrer
  3. waitto stand overnight
  4. temperaturecooled to -60° C.
  5. customresulting in a precipitate
  6. customThe precipitate was recrystallized from ether

出典と根拠

ORDレコード
ord-506e16f2806c491f9af80d5252fa702a
出典データセット
uspto-grants-1979_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04163112

反応ノート

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