Chlorosulfonic acid → p-[2-[(5-Chloro-2-methoxybenzoyl)amino]ethyl]benzenesulfonic Acid

HRID 1658597

반응식

HRID 1658597 반응식
[CH2:1]([NH:9][C:10](=[O:20])[C:11]1[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:12]=1[O:18][CH3:19])[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.Cl[S:22]([OH:25])(=[O:24])=[O:23]>C(Cl)(Cl)Cl>[Cl:17][C:15]1[CH:14]=[CH:13][C:12]([O:18][CH3:19])=[C:11]([CH:16]=1)[C:10]([NH:9][CH2:1][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([S:22]([OH:25])(=[O:24])=[O:23])=[CH:5][CH:4]=1)=[O:20]

참가 물질

4

반응물 2

HCID 24638Chlorosulfonic acidHCID 1185755-chloro-2-methoxy-N-(2-phenylethyl)benzamide

생성물 1

HCID 10044620p-[2-[(5-Chloro-2-methoxybenzoyl)amino]ethyl]benzenesulfonic Acid

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

N-phenethyl-5-chloro-2-methoxybenzamide (10 g.) dissolved in 25 ml. of chloroform was cooled to -10° and 19 g. of chlorosulfonic acid was added dropwise, maintaining the temperature at -10° to 0°. After the addition was complete the mixture was allowed to rise to room temperature and it was poured onto cracked ice. The crude sulfonic acid was filtered and 7.3 g. (57%) was obtained. A sample recrystallized for analysis from alcohol-acetonitrile melted at 188°-189°. Anal. Calcd. for C16H16ClNO5S: C, 51.94; H, 4.36; Cl, 9.58; N, 3.79; S, 8.67. Found: C, 50.10; H, 4.27; Cl, 9.93; N, 4.04; S, 8.84.

후처리

  1. temperaturemaintaining the temperature at -10° to 0°
  2. additionAfter the addition
  3. customto rise to room temperature
  4. additionit was poured
  5. filtrationThe crude sulfonic acid was filtered
  6. custom(57%) was obtained
  7. customA sample recrystallized for analysis from alcohol-acetonitrile melted at 188°-189°

출처 및 근거

ORD 기록
ord-bc8f02c5c844401397121a31c0651e41
출처 데이터셋
uspto-grants-1976_06
특허 번호
US03965173

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