Hydrochloric Acid → Benzyl cis(+/-)-[1-(1H-imidazol-1-ylcarbonothioyl)-3-methoxypiperidin-4-yl]-carbamate

HRID 43512

반응식

HRID 43512 반응식
[CH3:1][O:2][C@H:3]1[C@@H:8]([NH:9][C:10](=[O:19])[O:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:7][CH2:6][NH:5][CH2:4]1.[C:20](N1C=CN=C1)([N:22]1[CH:26]=[CH:25][N:24]=[CH:23]1)=[S:21].Cl>C1COCC1>[N:22]1([C:20]([N:5]2[CH2:6][CH2:7][C@H:8]([NH:9][C:10](=[O:19])[O:11][CH2:12][C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C@H:3]([O:2][CH3:1])[CH2:4]2)=[S:21])[CH:26]=[CH:25][N:24]=[CH:23]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 802641,1'-ThiocarbonyldiimidazoleHCID 86648490Benzyl cis(+/-)-[3-methoxypiperidin-4-yl]carbamate

생성물 1

HCID 86648520Benzyl cis(+/-)-[1-(1H-imidazol-1-ylcarbonothioyl)-3-methoxypiperidin-4-yl]-carbamate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Benzyl cis(±)-4-(3-methoxypiperidin-4-yl)-carbamate obtained by the method described in Example (40b) (735 mg, 1.37 mmol) was dissolved in THF (8 mL). 1,1′-Thiocarbonyldiimidazole (270 mg, 1.36 mmol) was added, and the mixture was stirred for 1.5 hours. 0.5 M hydrochloric acid was added to the reaction solution, followed by extraction with ethyl acetate and dichloromethane. The organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The resulting compound was used for the next reaction without purification.

후처리

  1. extractionfollowed by extraction with ethyl acetate and dichloromethane
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe resulting compound was used for the next reaction without purification

출처 및 근거

ORD 기록
ord-29d69e4f601b4ecbbaee4f6addca5f23
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536197B2

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