Hydrochloric Acid → HCID 86749750、化合物

HRID 1078718ノート

反応式

HRID 1078718 の反応式
C(OC([N:8]1[CH2:12][C@H:11]([O:13][Si](C(C)(C)C)(C)C)[CH2:10][C@H:9]1[C:21](=[O:27])[CH2:22][C:23](=[O:26])[NH:24][CH3:25])=O)(C)(C)C.[ClH:28]>CO>[ClH:28].[OH:13][C@H:11]1[CH2:12][NH:8][C@H:9]([C:21](=[O:27])[CH2:22][C:23](=[O:26])[NH:24][CH3:25])[CH2:10]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 22865011HCID 22865011、化合物

生成物 1

HCID 86749750HCID 86749750、化合物収率 62%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a solution of (2S,4R)-N-tert-butoxycarbonyl-4-tert-butyldimethylsiloxy-2-[2-(N-methylcarbamoyl)-1-oxoethyl]pyrrolidine (2.07 g, 5.3 mmol) in methanol (10 ml) was added a 5.5N hydrogen chloride--methanol solution (6 ml, 33 mmol). The mixture was stirred at room temperature for 6 h. The reaction solution was concentrated in vacuo. Tetrahydrofuran and ethanol were added to the obtained residue, and the precipitate was collected by filtration and washed with ethanol to obtain (2S,4R)-4-hydroxy-2-[2-(N-methylcarbamoyl)-1-oxoethyl]pyrrolidine monohydrochloride (737 mg, yield: 62%).

後処理

  1. concentrationThe reaction solution was concentrated in vacuo
  2. additionTetrahydrofuran and ethanol were added to the obtained residue
  3. filtrationthe precipitate was collected by filtration
  4. washwashed with ethanol

出典と根拠

ORDレコード
ord-67a4d905d8a94c0ea3c6fe07db6b2ca8
出典データセット
uspto-grants-1996_08
特許番号
US05550121

反応ノート

読み込み中…