Phosgene → o-sec-Butylphenyl chloroformate

HRID 2083263

반응식

HRID 2083263 반응식
[C:1]([Cl:4])(Cl)=[O:2].[CH:5]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[OH:15])([CH2:7][CH3:8])[CH3:6].CN(C)C(N(C)C)=O>>[CH:5]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[O:15][C:1]([Cl:4])=[O:2])([CH2:7][CH3:8])[CH3:6]

참가 물질

4

반응물 3

HCID 6371Phosgene3회HCID 69842-sec-ButylphenolHCID 12437Tetramethylurea

생성물 1

HCID 3016372o-sec-Butylphenyl chloroformate수율 97%

반응 조건

온도
100 °C

실험 절차

In a round flask provided with stirrer, thermometer, an introduction tube for phosgene and a reflux cooler operating at about -30° C a mixture of 150 g of o-sec.-butylphenol and 4 g of N,N,N',N',-tetramethyl urea was heated at 100° C and phosgene was introduced to such a degree that the phosgene reflux in the deep-freezing cooler did not increase so much as to reduce the sump temperature. After a reaction time of about 5 hours and a phosgene consumption of about 190 g the reflux cooler was replaced by a descending cooler so that the greatest part of the excess phosgene could be separated from the reaction mixture by distillation. The rest of phosgene was blown out with dry nitrogen. Thus, a yield of about 97% of chloroformic acid-o-sec.-butyl-phenyl-ester was obtained which was practically free from the starting product (GC).

후처리

  1. customIn a round flask provided with stirrer
  2. temperaturereflux in the deep-freezing cooler
  3. temperaturedid not increase so much as
  4. customAfter a reaction time of about 5 hours and a phosgene consumption of about 190 g the reflux cooler
  5. customcould be separated from the reaction mixture by distillation

출처 및 근거

ORD 기록
ord-0b051d0a67eb4ffab9a74e8ad4b9d465
출처 데이터셋
uspto-grants-1978_04
특허 번호
US04085129

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