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

HRID 67926ノート

反応式

HRID 67926 の反応式
[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

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 133730Flupropadine

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-78f022cad8e2421c9adf8015ee096779
出典データセット
uspto-grants-1982_08
特許番号
US04347252

反応ノート

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