2-Nitrobenzyl alcohol → o-Nitrobenzyl benzylcarbamate

HRID 399372

반응식

HRID 399372 반응식
[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:19]=[C:20]=[O:21])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>C1(C)C=CC=CC=1>[CH2:12]([NH:19][C:20](=[O:21])[O:7][CH2:6][C:5]1[CH:8]=[CH:9][CH:10]=[CH:11][C:4]=1[N+:1]([O-:3])=[O:2])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

참가 물질

4

반응물 2

HCID 119232-Nitrobenzyl alcoholHCID 76639Benzyl isocyanate

생성물 1

HCID 54357994o-Nitrobenzyl benzylcarbamate수율 67.9%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

10 ml of toluene, 5.75 g of 2-nitrobenzyl alcohol and 5 g of benzyl isocyanate were heated to reflux for 3 hours in a nitrogen atmosphere. Following cooling of the mixture, 50 ml of toluene was added. This reaction solution was washed several times with water, and was then dehydrated with sodium sulfate. The sodium sulfate was then filtered out, and the solvent was removed from the filtrate by means of a rotary evaporator. The solid obtained was recrystallized from a hexane-toluene mixed solvent, producing 7.3 g of o-nitrobenzyl benzylcarbamate in the form of plate yellow crystals. This compound had a melting point of 110° to 111° C., and the infrared absorption spectrum was 3308 cm-1 : N--H, 1696 cm-1 : C=O, 1520 cm-1 : N--O.

후처리

  1. temperatureto reflux for 3 hours in a nitrogen atmosphere
  2. additionwas added
  3. washThis reaction solution was washed several times with water
  4. filtrationThe sodium sulfate was then filtered out
  5. customthe solvent was removed from the filtrate by means of a rotary evaporator
  6. customThe solid obtained
  7. customwas recrystallized from a hexane-toluene mixed solvent

출처 및 근거

ORD 기록
ord-3298aea7a9fa46d480cf89f625cec7f6
출처 데이터셋
uspto-grants-1998_10
특허 번호
US05820944

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