Benzoic acid, 2-chloro-5-(chlorosulfonyl)- → HCID 20505864, 화합물

HRID 355121노트

반응식

HRID 355121 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([S:11](Cl)(=[O:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[Cl:15][C:16]1[CH:21]=[CH:20][C:19]([CH2:22][CH2:23][NH2:24])=[CH:18][CH:17]=1>C(Cl)Cl>[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([S:11]([NH:24][CH2:23][CH2:22][C:19]2[CH:20]=[CH:21][C:16]([Cl:15])=[CH:17][CH:18]=2)(=[O:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]

참가 물질

4

반응물 2

HCID 67306Benzoic acid, 2-chloro-5-(chlorosulfonyl)-HCID 674302-(4-Chlorophenyl)ethylamine

생성물 1

HCID 20505864HCID 20505864, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2-Chloro-5-chlorosulfonyl benzoic acid, 3.5 g. (0.014 mole), is added to a solution of 2-(p-chlorophenyl)ethylamine, 6.5 g. (0.042 mole) in 25 ml. methylene chloride. The resulting slurry is stirred overnight and filtered to recover 9.7 g. of residue. This is recrystallized three times from aqueous isopropanol, then dissolved in 1 N aqueous sodium hydroxide, washed three times with ether, and then acidified with conc. hydrochloric acid. The resulting precipitate is recrystallized twice from aqueous isopropanol to yield the desired product, m.p. 176°-178° C.

후처리

  1. filtrationfiltered
  2. customto recover 9.7 g
  3. customThis is recrystallized three times from aqueous isopropanol
  4. dissolutiondissolved in 1 N aqueous sodium hydroxide
  5. washwashed three times with ether
  6. customThe resulting precipitate is recrystallized twice from aqueous isopropanol

출처 및 근거

ORD 기록
ord-ae750f8829a0456dbba0ef8f8bf428a7
출처 데이터셋
uspto-grants-1983_03
특허 번호
US04377521

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