Triethylamine → 1-Benzyl 3-methyl azetidine-1,3-dicarboxylate

HRID 1958676ノート

反応式

HRID 1958676 の反応式
Cl.[CH3:2][O:3][C:4]([CH:6]1[CH2:9][NH:8][CH2:7]1)=[O:5].C(N(CC)CC)C.Cl[C:18]([O:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[O:19]>C(Cl)Cl>[N:8]1([C:18]([O:20][CH2:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[O:19])[CH2:9][CH:6]([C:4]([O:3][CH3:2])=[O:5])[CH2:7]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10387Benzyl chloroformateHCID 21100040Methyl azetidine-3-carboxylate hydrochloride

生成物 1

HCID 450725021-Benzyl 3-methyl azetidine-1,3-dicarboxylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

10 g of azetidine-3-carboxylic methyl ester hydrochloride and then 23 ml of triethylamine are added to 150 ml of CH2Cl2. The mixture is cooled and 13.5 g of benzyl chloroformate are added. After leaving overnight at AT, washing is carried out with water and then with HCl (N). After drying, concentrating to dryness and purifying by chromatography on silica (eluent: heptane-AcOEt (gradient from 0% to 50%)), 13.1 g of the expected compound are obtained.

後処理

  1. temperatureThe mixture is cooled
  2. customAfter leaving overnight at AT
  3. washwashing
  4. customAfter drying
  5. concentrationconcentrating to dryness
  6. custompurifying by chromatography on silica (eluent: heptane-AcOEt (gradient from 0% to 50%)), 13.1 g of the expected compound
  7. customare obtained

出典と根拠

ORDレコード
ord-5fd37fb0346845d19ef9c506ffa14fb7
出典データセット
uspto-grants-2013_04
特許番号
US08410137B2

反応ノート

読み込み中…