Hydrogen chloride-ethyl acetate → Benzyl benzyl[cis(+/-)-3-methoxypiperidin-4-yl]carbamate

HRID 43969노트

반응식

HRID 43969 반응식
Cl.C(OCC)(=O)C.[CH2:8]([N:15]([C:31]([O:33][CH2:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)=[O:32])[C@H:16]1[CH2:21][CH2:20][N:19](C(OC(C)(C)C)=O)[CH2:18][C@H:17]1[O:29][CH3:30])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>CO>[CH2:8]([N:15]([C@H:16]1[CH2:21][CH2:20][NH:19][CH2:18][C@H:17]1[O:29][CH3:30])[C:31](=[O:32])[O:33][CH2:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

참가 물질

4

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 86648850tert-Butyl cis(+/-)-4-{benzyl[(benzyloxy)carbonyl]amino}-3-methoxypiperidine-1-carboxylate

생성물 1

HCID 86712358Benzyl benzyl[cis(+/-)-3-methoxypiperidin-4-yl]carbamate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A 4 N hydrochloric acid/ethyl acetate solution (5 ml, 20 mmol) was added to a solution of tert-butyl cis(±)-4-{benzyl[(benzyloxy)carbonyl]amino}-3-methoxypiperidine-1-carboxylate obtained in Example (259b) (about 1.44 mmol) in methanol (1 mL). The mixture was stirred for one hour and the solvent was evaporated under reduced pressure. The reaction solution was diluted with ethyl acetate, washed with aqueous sodium bicarbonate solution and brine, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The resulting compound was used for the next reaction without purification.

후처리

  1. customthe solvent was evaporated under reduced pressure
  2. additionThe reaction solution was diluted with ethyl acetate
  3. washwashed with aqueous sodium bicarbonate solution and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting compound was used for the next reaction without purification

출처 및 근거

ORD 기록
ord-8c53541dcea1496f87d3bb6c2433f89e
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536197B2

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