Water → HCID 67048682, 화합물

HRID 551221

반응식

HRID 551221 반응식
[Cl:1][C:2]1[CH:8]=[C:7]([CH3:9])[CH:6]=[CH:5][C:3]=1[NH2:4].[Cl:10][CH2:11][CH2:12][CH2:13][CH2:14][S:15](Cl)(=[O:17])=[O:16].O>N1C=CC=CC=1>[Cl:1][C:2]1[CH:8]=[C:7]([CH3:9])[CH:6]=[CH:5][C:3]=1[NH:4][S:15]([CH2:14][CH2:13][CH2:12][CH2:11][Cl:10])(=[O:17])=[O:16]

참가 물질

5

반응물 3

HCID 962WaterHCID 120072-Chloro-p-toluidineHCID 742124-Chlorobutane-1-sulphonyl chloride

생성물 1

HCID 67048682HCID 67048682, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

1.30 ml (10.7 mmol) 2-chloro-4-methyl-aniline are placed in 30 ml of pyridine, combined with 2.67 g (10.5 mmol) 75% m 4-chlorobutyl-sulphonic acid chloride and stirred for 16 hours at ambient temperature. The reaction mixture is poured into water and extracted with ethyl acetate. The combined organic phases are washed with 6-molar hydrochloric acid, dried over sodium sulphate and evaporated down i. vac. The residue is purified by chromatography on silica gel (eluting gradient: petroleum ether/ethyl acetate=9:1→7:3).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe combined organic phases are washed with 6-molar hydrochloric acid
  3. dry with materialdried over sodium sulphate
  4. customevaporated down i
  5. customThe residue is purified by chromatography on silica gel (eluting gradient: petroleum ether/ethyl acetate=9:1→7:3)

출처 및 근거

ORD 기록
ord-4d703f5426c44af6b1c1cde516e6e502
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07947700B2

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