Methanesulfonic Acid → 1-(3,5-Bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne methanesulphonate

HRID 67926노트

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HRID 67926 반응식
[F:1][C:2]([F:27])([F:26])[C:3]1[CH:4]=[C:5]([C:13]#[C:14][CH2:15][N:16]2[CH2:21][CH2:20][CH:19]([C:22]([CH3:25])([CH3:24])[CH3:23])[CH2:18][CH2:17]2)[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.[CH3:28][S:29]([OH:32])(=[O:31])=[O:30]>C(OCC)C>[CH3:28][S:29]([OH:32])(=[O:31])=[O:30].[F:12][C:9]([F:10])([F:11])[C:7]1[CH:6]=[C:5]([C:13]#[C:14][CH2:15][N:16]2[CH2:17][CH2:18][CH:19]([C:22]([CH3:23])([CH3:24])[CH3:25])[CH2:20][CH2:21]2)[CH:4]=[C:3]([C:2]([F:26])([F:27])[F:1])[CH:8]=1

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 133730Flupropadine

생성물 1

HCID 205264891-(3,5-Bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne methanesulphonate수율 95.4%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A solution of 1-(3,5-bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne (9.78 g) in anhydrous diethyl ether (12.5 ml) was treated with a solution of methanesulphonic acid (2.40 g) in anhydrous diethyl ether (12.5 ml), stirred and cooled. The solid precipitate was removed by filtration, washed with cold anhydrous diethyl ether and dried at 0.05 mm Hg for 2 hours, to give 1-(3,5-bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne methanesulphonate (11.61 g), m.p. 164°-165° C., in the form of a white powder which had the elementary analysis C: 51.3%; H: 5.49%; N: 2.60% (C21H27F6NO3S requires C: 51.73%; H: 5.58%; N: 2.87%).

후처리

  1. temperaturecooled
  2. customThe solid precipitate was removed by filtration
  3. washwashed with cold anhydrous diethyl ether
  4. customdried at 0.05 mm Hg for 2 hours

출처 및 근거

ORD 기록
ord-78f022cad8e2421c9adf8015ee096779
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04347252

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