Methyl iodide → methyl 4-[4-(4,5-dihydro-5-phenyl-3-isoxazolyl)-2-thiazolyl]-N-(2,5-dimethylphenyl)-1-piperidinecarboximidothioate

HRID 1802320노트

반응식

HRID 1802320 반응식
[C:1]1([CH:7]2[O:11][N:10]=[C:9]([C:12]3[N:13]=[C:14]([CH:17]4[CH2:22][CH2:21][N:20]([C:23](=[S:33])[NH:24][C:25]5[CH:30]=[C:29]([CH3:31])[CH:28]=[CH:27][C:26]=5[CH3:32])[CH2:19][CH2:18]4)[S:15][CH:16]=3)[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:34]I>ClCCl>[C:1]1([CH:7]2[O:11][N:10]=[C:9]([C:12]3[N:13]=[C:14]([CH:17]4[CH2:18][CH2:19][N:20]([C:23]([S:33][CH3:34])=[N:24][C:25]5[CH:30]=[C:29]([CH3:31])[CH:28]=[CH:27][C:26]=5[CH3:32])[CH2:21][CH2:22]4)[S:15][CH:16]=3)[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

4

반응물 2

HCID 6328Methyl iodideHCID 866476744-[4-(4,5-dihydro-5-phenyl-3-isoxazolyl)-2-thiazolyl]-N-(2,5-dimethylphenyl)-1-piperidinecarbothioamide

생성물 1

HCID 66633932methyl 4-[4-(4,5-dihydro-5-phenyl-3-isoxazolyl)-2-thiazolyl]-N-(2,5-dimethylphenyl)-1-piperidinecarboximidothioate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 14-[4-(4,5-dihydro-5-phenyl-3-isoxazolyl)-2-thiazolyl]-N-(2,5-dimethylphenyl)-1-piperidinecarbothioamide (i.e. the product of Step C) (476 mg, 1.0 mmol) and methyl iodide (0.25 mL, 4.0 mmol) in dichloromethane (2 mL) was agitated at room temperature for 3 h. The reaction mixture was then diluted with dichloromethane, washed with saturated aqueous sodium bicarbonate, saturated aqueous sodium chloride, dried (MgSO4), and concentrated to give a foamy white solid (480 mg). The solid was crystallized from methyl acetate/petroleum ether to give the title compound, a compound of the present invention, as a white powder (320 mg) melting at 114-116° C.

후처리

  1. washwashed with saturated aqueous sodium bicarbonate, saturated aqueous sodium chloride
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ec8bfcb6433e49808bfa34eeb8166d8f
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08349870B2

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