Morpholine → 2-Methyl-2-morpholino-1-(4-piperidinophenyl)-propan-1-one

HRID 981756노트

반응식

HRID 981756 반응식
[CH3:1][C:2]1([CH3:19])O[C:3]1([O:17]C)[C:5]1[CH:10]=[CH:9][C:8]([N:11]2[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)=[CH:7][CH:6]=1.[NH:20]1[CH2:25][CH2:24][O:23][CH2:22][CH2:21]1>>[CH3:19][C:2]([N:20]1[CH2:25][CH2:24][O:23][CH2:22][CH2:21]1)([CH3:1])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([N:11]2[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)=[CH:7][CH:6]=1)=[O:17]

참가 물질

3

반응물 2

HCID 8083MorpholineHCID 198794483,3-Dimethyl-2-methoxy-2-(4-piperidinophenyl)-oxirane

생성물 1

HCID 198794392-Methyl-2-morpholino-1-(4-piperidinophenyl)-propan-1-one

반응 조건

온도
130 °C

실험 절차

12.1 g (46.3 mmol) of 3,3-dimethyl-2-methoxy-2-(4-piperidinophenyl)-oxirane and 26.1 g (0.30 mol) of morpholine are added together, and the mixture is heated to the refluxing temperature (about 130° C.). After 6 hours the mixture is cooled down and the morpholine is distilled off under reduced pressure. The residue is taken up in toluene and is extracted with dilute hydrochloric acid. The hydrochloric acid solution is rendered alkaline and is extracted with toluene. The toluene solution is dried with K2CO3 and concentrated. The residue is recrystallised from methanol. Melting point 159°-162° C.

후처리

  1. temperatureAfter 6 hours the mixture is cooled down
  2. distillationthe morpholine is distilled off under reduced pressure
  3. extractionis extracted with dilute hydrochloric acid
  4. extractionis extracted with toluene
  5. dry with materialThe toluene solution is dried with K2CO3
  6. concentrationconcentrated
  7. customThe residue is recrystallised from methanol

출처 및 근거

ORD 기록
ord-8fef067ad98d4232add3817460531d19
출처 데이터셋
uspto-grants-1991_02
특허 번호
US04992547

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