4-Nitrobenzenesulfonic acid → Nosyl ether

HRID 1252767

반응식

HRID 1252767 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10]([OH:13])(=[O:12])=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>ClC=CCl>[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([S:10]([O:13][S:10]([C:7]2[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:9][CH:8]=2)(=[O:11])=[O:12])(=[O:11])=[O:12])=[CH:8][CH:9]=1)([O-:3])=[O:2]

참가 물질

4

반응물 2

HCID 87404-Nitrobenzenesulfonic acidHCID 14812Phosphorus oxide (P4O10)

생성물 1

HCID 13084338Nosyl ether수율 20.9%

시약·촉매·용매 1

HCID 109001,2-Dichloroethylene용매

실험 절차

A mixture of p-nitrobenzensulfonic acid (20 g), phosphorous pentoxide (50 g) and 1,2-dichloroethylene (100 ml) is heated at reflux for 4 days. The hot supernatant is decanted from the gummy residue and allowed to cool to room temperature. The resulting crystalline precipitate of p-nitrobenzenesulfonic anhydride (1.5 g) is collected, washed with anhydrous diethylether, and dried under vacuum. The gummy residue is twice more refluxed overnight with 100 ml portions of dichloroethylene and worked up as above to provide additional p-nitrobenzenesulfonic anhydride (4.0 g); mp 171°-172°.

후처리

  1. temperatureis heated
  2. temperatureat reflux for 4 days
  3. customThe hot supernatant is decanted from the gummy residue
  4. customThe resulting crystalline precipitate of p-nitrobenzenesulfonic anhydride (1.5 g) is collected
  5. washwashed with anhydrous diethylether
  6. customdried under vacuum
  7. temperatureThe gummy residue is twice more refluxed overnight with 100 ml portions of dichloroethylene

출처 및 근거

ORD 기록
ord-a0f43e6085174fc7a9fb6bcda8e73089
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04745188

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