Phosgene → 2-(1-Methoxycarbonylethoxy)benzenesulfonyl isocyanate

HRID 4486

反応式

HRID 4486 の反応式
[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]

参加物

6

反応物 3

HCID 6371Phosgene2 回HCID 8110Butyl isocyanateHCID 221528372-(1-Methoxycarbonylethoxy)benzenesulfonamide

生成物 1

HCID 221528362-(1-Methoxycarbonylethoxy)benzenesulfonyl isocyanate収率 125.5%

試薬・触媒・溶媒 2

HCID 66583054Diazabicyclooctane触媒HCID 7237O-Xylene溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-256cd9153e88410d975da315b2913afe
出典データセット
uspto-grants-1988_02
特許番号
US04726836

関連ノート

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