Triethylamine → 1-(4-Methoxypiperidinosulphonyl)-4-nitro-2-trifluoromethyl-benzene

HRID 1076650노트

반응식

HRID 1076650 반응식
C(N(CC)CC)C.[CH3:8][O:9][CH:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1.[N+:16]([C:19]1[CH:24]=[CH:23][C:22]([S:25](Cl)(=[O:27])=[O:26])=[C:21]([C:29]([F:32])([F:31])[F:30])[CH:20]=1)([O-:18])=[O:17]>C(Cl)Cl>[CH3:8][O:9][CH:10]1[CH2:15][CH2:14][N:13]([S:25]([C:22]2[CH:23]=[CH:24][C:19]([N+:16]([O-:18])=[O:17])=[CH:20][C:21]=2[C:29]([F:30])([F:31])[F:32])(=[O:27])=[O:26])[CH2:12][CH2:11]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 776664-MethoxypiperidineHCID 108034044-Nitro-2-(trifluoromethyl)benzene-1-sulfonyl chloride

생성물 1

HCID 215191911-(4-Methoxypiperidinosulphonyl)-4-nitro-2-trifluoromethyl-benzene

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
25 °C

실험 절차

Triethylamine (1.0 g) and 4-methoxypiperidine (1.15 g) were added to a solution of 4-nitro-2-trifluoromethyl-benzene sulphonyl chloride (2.89 g) in methylene chloride (40 ml). The mixture was stirred at 25°C. for 2 hours and then evaporated to dryness in vacuo. The residual oil was triturated with 1:1 aqueous isopropanol and the resulting solid was recrystallized from isopropanol to give 1-(4-methoxypiperidinosulphonyl)-4-nitro-2-trifluoromethyl-benzene, m.p. 141°-143°C.

후처리

  1. customevaporated to dryness in vacuo
  2. customThe residual oil was triturated with 1:1 aqueous isopropanol
  3. customthe resulting solid was recrystallized from isopropanol

출처 및 근거

ORD 기록
ord-ffaae18a234b4a4abae1ee20adf78dda
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03957796

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