1,1'-Thiocarbonyldiimidazole → cis(+/-)-4-Chloro-5-ethyl-N-[1-(1H-imidazol-1-ylcarbonothioyl)-3-methoxypiperidin-4-yl]-1H-imidazole-2-carboxamide

HRID 43518노트

반응식

HRID 43518 반응식
[Cl:1][C:2]1[N:3]=[C:4]([C:9]([NH:11][C@H:12]2CCN(C(OC(C)(C)C)=O)C[C@H]2OC)=[O:10])[NH:5][C:6]=1[CH2:7][CH3:8].Cl.[C:28]([O:31][CH2:32][CH3:33])(=O)C.[C:34]([N:41]1[CH:45]=[CH:44]N=C1)([N:36]1[CH:40]=[CH:39][N:38]=[CH:37]1)=[S:35]>CO>[Cl:1][C:2]1[N:3]=[C:4]([C:9]([NH:11][C@H:12]2[CH2:44][CH2:45][N:41]([C:34]([N:36]3[CH:40]=[CH:39][N:38]=[CH:37]3)=[S:35])[CH2:33][C@H:32]2[O:31][CH3:28])=[O:10])[NH:5][C:6]=1[CH2:7][CH3:8]

참가 물질

5

반응물 3

HCID 802641,1'-ThiocarbonyldiimidazoleHCID 21866389Hydrogen chloride-ethyl acetateHCID 86648452tert-Butyl cis(+/-)-4-{[(4-chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}-3-methoxypiperidine-1-carboxylate

생성물 1

HCID 86648525cis(+/-)-4-Chloro-5-ethyl-N-[1-(1H-imidazol-1-ylcarbonothioyl)-3-methoxypiperidin-4-yl]-1H-imidazole-2-carboxamide

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

tert-Butyl cis(±)-4-{[(4-chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}-3-methoxypiperidine-1-carboxylate obtained by the method described in Example (1g) (130 mg, 0.34 mmol) was dissolved in methanol (1 mL). A 4 N hydrochloric acid/ethyl acetate solution (3 mL) was added, and the mixture was stirred for 15 minutes. The reaction solution was concentrated under reduced pressure, and then the same operation as in Example (64a) was performed using 1,1′-thiocarbonyldiimidazole (81 mg, 0.45 mmol), to obtain the title compound. The resulting compound was used for the next reaction without purification.

후처리

  1. concentrationThe reaction solution was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0746a1d343cd4867831732b6b970cdc4
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536197B2

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