3,5-Diiodosalicylic acid → Rafoxanide

HRID 1076350

반응식

HRID 1076350 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5](C2C=CC(Cl)=CC=2)=[C:4]([Cl:15])[CH:3]=1.CC[O:18][CH2:19][CH3:20].[I:21][C:22]1[CH:30]=[C:29]([I:31])[CH:28]=[C:24]([C:25]([OH:27])=O)[C:23]=1[OH:32].P(Cl)(Cl)Cl>ClC1C=CC=CC=1>[I:21][C:22]1[CH:30]=[C:29]([I:31])[CH:28]=[C:24]([C:25]([NH:1][C:2]2[CH:7]=[CH:6][C:5]([O:18][C:19]3[CH:20]=[CH:5][C:4]([Cl:15])=[CH:3][CH:2]=3)=[C:4]([Cl:15])[CH:3]=2)=[O:27])[C:23]=1[OH:32]

참가 물질

5

반응물 3

HCID 86313,5-Diiodosalicylic acidHCID 24387Phosphorus trichlorideHCID 68128298HCID 68128298, 화합물

생성물 1

HCID 31475Rafoxanide

시약·촉매·용매 1

HCID 7964Chlorobenzene용매

실험 절차

A mixture of 31.0 g. of 4-amino-2,4'-dichlorobiphenyl ether, 47.4 g. of 3,5-diiodo salicylic acid, and 4.3 ml. of phosphorus trichloride in 235 ml. of chlorobenzene is refluxed for 3 hours. The hot solution is decanted from some insoluble residue and the crude product settles out of solution upon cooling to room temperature. Upon recrystallization from benzene, 27.8 g. of 3,5-diiodo-3'-chloro-4'-(p-chlorophenoxy)-salicylanilide, m.p. 168°-170°C. is obtained.

후처리

  1. additionA mixture of 31.0 g
  2. customThe hot solution is decanted from some insoluble residue
  3. customUpon recrystallization from benzene, 27.8 g

출처 및 근거

ORD 기록
ord-11d59ee90d08415d8557772cd75a0a21
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03956488

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