2-Nitrobenzyl alcohol → o-Nitrobenzyl n-octylcarbamate

HRID 343268

反応式

HRID 343268 の反応式
[N+:1]([C:4]1[CH:11]=[CH:10][CH:9]=[CH:8][C:5]=1[CH2:6][OH:7])([O-:3])=[O:2].[CH2:12]([N:20]=[C:21]=[O:22])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19]>C1(C)C=CC=CC=1>[CH2:12]([NH:20][C:21](=[O:22])[O:7][CH2:6][C:5]1[CH:8]=[CH:9][CH:10]=[CH:11][C:4]=1[N+:1]([O-:3])=[O:2])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19]

参加物

4

反応物 2

HCID 119232-Nitrobenzyl alcoholHCID 76616Octyl isocyanate

生成物 1

HCID 18695120o-Nitrobenzyl n-octylcarbamate収率 62.1%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

100 mL toluene, 10 g 2-nitrobenzyl alcohol, and 11.4 g octyl isocyanate were placed in a 200-mL roundbottom flask, heated at reflux under nitrogen for 2 hours, and then cooled. The reaction solution was washed with water several times and the resulting toluene solution was then dried over sodium sulfate. The sodium sulfate was filtered off and the solvent was removed from the filtrate on a rotary evaporator. The resulting solid was recrystallized twice from hexane, yielding 12.5 g o-nitrobenzyl n-octylcarbamate as light yellow needle-like crystals.

後処理

  1. temperatureheated
  2. temperatureat reflux under nitrogen for 2 hours
  3. temperaturecooled
  4. washThe reaction solution was washed with water several times
  5. dry with materialthe resulting toluene solution was then dried over sodium sulfate
  6. filtrationThe sodium sulfate was filtered off
  7. customthe solvent was removed from the filtrate on a rotary evaporator
  8. customThe resulting solid was recrystallized twice from hexane

出典と根拠

ORDレコード
ord-c1509082ca37431e9befdb5f19a240a9
出典データセット
uspto-grants-1999_01
特許番号
US05861235

関連ノート

読み込み中…