Butyl isocyanate → HCID 19973469, 화합물

HRID 1452056노트

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HRID 1452056 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH2:11])(=[O:10])=[O:9])=[C:4]([Cl:12])[CH:3]=1.C(N=[C:18]=[O:19])CCC.C(Cl)(=O)[C:21](Cl)=[O:22]>ClC1C=CC=CC=1>[Cl:12][C:4]1[CH:3]=[C:2]([N:1]=[C:21]=[O:22])[CH:7]=[CH:6][C:5]=1[S:8]([N:11]=[C:18]=[O:19])(=[O:9])=[O:10]

참가 물질

5

반응물 3

HCID 8110Butyl isocyanateHCID 65578Oxalyl chlorideHCID 125335224-Amino-2-chlorobenzene-1-sulfonamide

생성물 1

HCID 19973469HCID 19973469, 화합물

시약·촉매·용매 1

HCID 7964Chlorobenzene용매

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온도
100 °C

실험 절차

5,7-Dichloro-4-[4-(methylcarbamoyl)-2-chlorobenzenesulfonimide]-1,4-dihydroquinoline-2-carboxylic acid, methyl ester ##STR39## Dissolve 4-amino-2-chlorobenzenesulfonamide (0.96g, 5mmol) in chlorobenzene (10% solution) and distill the mixture to remove any traces of water. Cool to 100° C. and add n-butyl isocyanate (99mg, 1mmol). Heat to reflux and add, by dropwise addition, oxalyl chloride (1.5mL). Purge with nitrogen at 130°-132° C. for 30 minutes and distill to give 2-chloro-4-isocyanatobenzenesulfonyl isocyanate.

후처리

  1. distillationdistill the mixture
  2. customto remove any traces of water
  3. temperatureHeat
  4. temperatureto reflux
  5. customPurge with nitrogen at 130°-132° C. for 30 minutes
  6. distillationdistill

출처 및 근거

ORD 기록
ord-81bc4a6927634069912ccbdbe59be8e4
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05606063

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