Methanol → Methyl 3-Morpholinecarboxylate

HRID 1650132

反応式

HRID 1650132 の反応式
Cl.[NH:2]1[CH2:7][CH2:6][O:5][CH2:4][CH:3]1[C:8]([OH:10])=[O:9].S(Cl)(Cl)=O.[CH3:15]O>>[NH:2]1[CH2:7][CH2:6][O:5][CH2:4][CH:3]1[C:8]([O:10][CH3:15])=[O:9]

参加物

4

反応物 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 45790954Morpholine-3-carboxylic acid hydrochloride

生成物 1

HCID 3286806Methyl 3-Morpholinecarboxylate

反応条件

温度
-20 °C

実験手順

Morpholine-3-carboxylic acid hydrochloride (1.04 g) was dissolved in methanol (20 ml) and the solution cooled to -20° C. Thionyl chloride (1 ml) was added dropwise to the stirred reaction mixture such that the temperature did not rise above -10°. After the addition was complete the reaction mixture was stirred at room temperature for 16 h. The solvent was removed in vacuo and the resultant pale grey residue was partitioned between 2N Na2CO3 and dichloromethane. The organic phase was separated, dried, and the solvent was removed in vacuo to give the title compound as an oil (220 mg).

後処理

  1. customdid not rise above -10°
  2. additionAfter the addition
  3. customThe solvent was removed in vacuo
  4. customthe resultant pale grey residue was partitioned between 2N Na2CO3 and dichloromethane
  5. customThe organic phase was separated
  6. customdried
  7. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-6ca88673f4a8479ba37ac558ea48ddd5
出典データセット
uspto-grants-1990_05
特許番号
US04923863

関連ノート

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