Isethionic Acid → 1-(3,5-Bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne 2-hydroxyethanesulphonate

HRID 67927

반응식

HRID 67927 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.[OH:28][CH2:29][CH2:30][S:31]([OH:34])(=[O:33])=[O:32]>C(OCC)(=O)C>[OH:28][CH2:29][CH2:30][S:31]([OH:34])(=[O:33])=[O:32].[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 7866Isethionic AcidHCID 133730Flupropadine

생성물 1

HCID 127998631-(3,5-Bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne 2-hydroxyethanesulphonate수율 1,475.7%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

A solution of 1-(3,5-bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne (6.1 g) in ethyl acetate (20 ml) was treated with 2-hydroxyethanesulphonic acid (2.19 g) in ethyl acetate (20 ml). Evaporation of the solvent gave a waxy solid, m.p. 107°-109° C., which was recrystallised from a mixture of ethyl acetate and diethyl ether to give 1-(3,5-bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne 2-hydroxyethanesulphonate (containing 0.23 mole of water of crystallization) (5.61 g), m.p. 118°-119° C., in the form of a white crystalline solid which had the elementary analysis C: 50.3%; H: 6.05%; N: 2.68%; H2O: 0.8% (C22H29F6NO4S. 0.23 H2O requires C: 50.64%; H: 5.65%; N: 2.68%; H2O: 0.8%).

후처리

  1. customEvaporation of the solvent
  2. customgave a waxy solid, m.p. 107°-109° C., which
  3. customwas recrystallised from a mixture of ethyl acetate and diethyl ether

출처 및 근거

ORD 기록
ord-0ac830d9c8d34edbb9e5602040ce9440
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04347252

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