Phenol → Phenyl 2,4-dichloro-3-nitrobenzenesulfonate

HRID 840568

반응식

HRID 840568 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[N+:9]([O-:11])=[O:10].Cl[S:13]([OH:16])(=[O:15])=[O:14].[C:17]1(O)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C(N(CC)CC)C>CC(C)=O.O>[Cl:1][C:2]1[C:3]([N+:9]([O-:11])=[O:10])=[C:4]([Cl:8])[CH:5]=[CH:6][C:7]=1[S:13]([O:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)(=[O:15])=[O:14]

참가 물질

7

반응물 4

HCID 996PhenolHCID 8471TriethylamineHCID 117591,3-Dichloro-2-nitrobenzeneHCID 24638Chlorosulfonic acid2회

생성물 1

HCID 22619793Phenyl 2,4-dichloro-3-nitrobenzenesulfonate

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

2,6-Dichloronitrobenzene was stirred for 7 hours at 130° C. with an excess of chlorosulfonic acid. After cooling, the mixture was poured onto ice, the sulfochloride was filtered off with suction, washed to neutrality and dried over sodium hydroxide, melting point 91° C. The resulting sulfochloride (29.05 g, 0.1 mol) and phenol (11.5 g, 0.12 mol) were dissolved in 150 ml of acetone and treated with 14 ml of triethylamine at 10° C. The mixture was stirred for 1 hour with cooling, stirring was then continued for a further 4 hours at room temperature, the mixture was then treated with 200 ml of water, the resulting precipitate was filtered off with suction at 10° C., washed with water and dried in vacuo at 80° C., melting point 102° C.

후처리

  1. temperatureAfter cooling
  2. additionthe mixture was poured onto ice
  3. filtrationthe sulfochloride was filtered off with suction
  4. washwashed to neutrality
  5. dry with materialdried over sodium hydroxide, melting point 91° C
  6. temperaturewith cooling
  7. stirringstirring
  8. waitwas then continued for a further 4 hours at room temperature
  9. filtrationthe resulting precipitate was filtered off with suction at 10° C.
  10. washwashed with water
  11. customdried in vacuo at 80° C.

출처 및 근거

ORD 기록
ord-234ce935a86f4124aff4fc9e10c4bde2
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06369057B1

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