Ethyl chloroacetate → Ethyl 2-Morpholinoacetate

HRID 64076ノート

反応式

HRID 64076 の反応式
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.C([O-])([O-])=O.[K+].[K+].Cl[CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16]>CN(C=O)C>[O:4]1[CH2:5][CH2:6][N:1]([CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:2][CH2:3]1

参加物

5

反応物 3

HCID 7751Ethyl chloroacetateHCID 8083MorpholineHCID 11430Potassium Carbonate

生成物 1

HCID 2734105Ethyl 2-Morpholinoacetate収率 73.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of morpholine (0.5 g, 5.739 mmol, 1.0 eq) in DMF were added K2CO3 (1.98 g, 14.34 mmol, 2.5 eq.) and ethyl 2-chloroacetate (1.05 g, 8.60 mmol, 1.5 eq.). The mixture was stirred at RT for 12 h. The mixture was quenched and extracted as in Intermediate Example 5(a). The solvent was distilled off to afford the product in 73.9% yield (0.735 g). LC-MS (ESI): Calculated mass: 173.21; Observed mass 174.0 [M+H]+ (rt: 0.1-0.4 min).

後処理

  1. customThe mixture was quenched
  2. extractionextracted as in Intermediate Example 5(a)
  3. distillationThe solvent was distilled off
  4. customto afford the product in 73.9% yield (0.735 g)
  5. customObserved mass 174.0 [M+H]+ (rt: 0.1-0.4 min)

出典と根拠

ORDレコード
ord-bfdce75122a84f659de3c1baab96175c
出典データセット
uspto-grants-2016_09
特許番号
US09447091B2

反応ノート

読み込み中…