Phosgene → 2-(1-Methoxycarbonylethoxy)benzenesulfonyl isocyanate

HRID 4486

반응식

HRID 4486 반응식
[CH3:1][O:2][C:3]([CH:5]([O:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[S:14]([NH2:17])(=[O:16])=[O:15])[CH3:6])=[O:4].C(N=[C:23]=[O:24])CCC.C(Cl)(Cl)=O>N1(C2CCCCCCC2)CCCCCCN1.C1(C)C(C)=CC=CC=1>[CH3:1][O:2][C:3]([CH:5]([O:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[S:14]([N:17]=[C:23]=[O:24])(=[O:16])=[O:15])[CH3:6])=[O:4]

참가 물질

6

반응물 3

HCID 6371Phosgene2회HCID 8110Butyl isocyanateHCID 221528372-(1-Methoxycarbonylethoxy)benzenesulfonamide

생성물 1

HCID 221528362-(1-Methoxycarbonylethoxy)benzenesulfonyl isocyanate수율 125.5%

시약·촉매·용매 2

HCID 66583054Diazabicyclooctane촉매HCID 7237O-Xylene용매

실험 절차

A mixture of 12.9 g of 2-(1-methoxycarbonylethoxy)-benzenesulfonamide, 4.9 g of n-butylisocyanate and 0.1 g of diazabicyclooctane and 130 ml of xylene is refluxed for 30 minutes. Then 10 g of phosgene are passed into the solution at the same temperature over 90 minutes. Excess phosgene is expelled with nitrogen and the solution is then cooled and concentrated in vacuo, affording 17.7 g of 2-(1-methoxycarbonylethoxy)benzenesulfonyl isocyanate in the form of a brownish oil which can be further used without purification.

후처리

  1. temperatureis refluxed for 30 minutes
  2. temperaturethe solution is then cooled
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-256cd9153e88410d975da315b2913afe
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04726836

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