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

HRID 1885651노트

반응식

HRID 1885651 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>C1(C)C=CC=CC=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

4

반응물 2

HCID 8083Morpholine2회HCID 198794483,3-Dimethyl-2-methoxy-2-(4-piperidinophenyl)-oxirane

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

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 dissolved 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. extractionis extracted with dilute hydrochloric acid
  3. extractionis extracted with toluene
  4. dry with materialThe toluene solution is dried with K2CO3
  5. concentrationconcentrated
  6. customThe residue is recrystallised from methanol

출처 및 근거

ORD 기록
ord-bd986129cd9e4a40a670d5dace2405db
출처 데이터셋
uspto-grants-1992_09
특허 번호
US05145885

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