Water → Benzyl 3-hydroxypyrrolidine-1-carboxylate

HRID 374809ノート

反応式

HRID 374809 の反応式
[NH:1]1[CH2:5][CH2:4][CH:3]([OH:6])[CH2:2]1.[CH2:7]([O:14][C:15](Cl)=[O:16])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O>C(Cl)(Cl)Cl.C(N(CC)CC)C>[CH2:7]([O:14][C:15]([N:1]1[CH2:5][CH2:4][CH:3]([OH:6])[CH2:2]1)=[O:16])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

参加物

6

反応物 3

HCID 962WaterHCID 10387Benzyl chloroformateHCID 982104-Hydroxypyrrolidine

生成物 1

HCID 560953Benzyl 3-hydroxypyrrolidine-1-carboxylate

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 8471Triethylamine溶媒

実験手順

30 g of 3-pyrrolidinol was dissolved in 500 ml of chloroform, to which 53 ml of triethylamine was added, followed by gradually dropping 52 ml of benzyloxycarbonyl chloride at room temperature. After completion of the reaction, the reaction solution was poured into water and extracted with chloroform. The solvent was distilled off under reduced pressure and the resultant residue was purified by column chromatography (eluting solvent: hexane-ethyl acetate) to obtain 70.67 g of the intended compound.

後処理

  1. additionwas added
  2. customat room temperature
  3. customAfter completion of the reaction
  4. extractionextracted with chloroform
  5. distillationThe solvent was distilled off under reduced pressure
  6. customthe resultant residue was purified by column chromatography (eluting solvent: hexane-ethyl acetate)

出典と根拠

ORDレコード
ord-622ec98462384e448b3f2b77ee2bbe73
出典データセット
uspto-grants-1996_01
特許番号
US05482937

反応ノート

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