Methanol → Methyl 3-Morpholinecarboxylate

HRID 1650132

반응식

HRID 1650132 반응식
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]

참가 물질

4

반응물 3

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

생성물 1

HCID 3286806Methyl 3-Morpholinecarboxylate

반응 조건

온도
-20 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-6ca88673f4a8479ba37ac558ea48ddd5
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04923863

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