N-[2,6-Bis(1-methylethyl)-4-phenoxyphenyl]thiourea → 2-Isothiocyanato-1,3-bis(1-methylethyl)-5-phenoxybenzene

HRID 358833

반응식

HRID 358833 반응식
[O:1]([C:8]1[CH:13]=[C:12]([CH:14]([CH3:16])[CH3:15])[C:11]([NH:17][C:18](N)=[S:19])=[C:10]([CH:21]([CH3:23])[CH3:22])[CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>CC1C=CC=CC=1C>[O:1]([C:8]1[CH:13]=[C:12]([CH:14]([CH3:16])[CH3:15])[C:11]([N:17]=[C:18]=[S:19])=[C:10]([CH:21]([CH3:23])[CH3:22])[CH:9]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

3

반응물 1

HCID 15753006N-[2,6-Bis(1-methylethyl)-4-phenoxyphenyl]thiourea

생성물 1

HCID 132721472-Isothiocyanato-1,3-bis(1-methylethyl)-5-phenoxybenzene수율 93%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

315 g (1 mol) of N-(4-phenoxy-2,6-diisopropylphenyl)thiourea are suspended in 800 ml of o-xylene, and the suspension is heated for 5 hours to reflux temperature, whereupon the temperature of the reaction mixture rises to ca. 150° C. The reaction mixture is then cooled, the solvent is removed by vacuum distillation, and the crude product is purified by distillation under a high vacuum, giving 278 g (93% of theory) of 4-phenoxy-2,6-diisopropylphenylisothiocyanate as a pale yellow oil with a boiling point of 130°-140° C./0.05 mbar.

후처리

  1. temperaturethe suspension is heated for 5 hours
  2. temperatureto reflux temperature
  3. customrises to ca. 150° C
  4. temperatureThe reaction mixture is then cooled
  5. customthe solvent is removed by vacuum distillation
  6. distillationthe crude product is purified by distillation under a high vacuum

출처 및 근거

ORD 기록
ord-8db00d60bf8844a283dd11daf73c5577
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04997967

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