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

HRID 43969ノート

反応式

HRID 43969 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8c53541dcea1496f87d3bb6c2433f89e
出典データセット
uspto-grants-2013_09
特許番号
US08536197B2

反応ノート

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