Water → 2-Chloro-4-methyl-6-morpholino-pyridine-3-carboxylic acid methylester

HRID 1039781노트

반응식

HRID 1039781 반응식
[CH3:1][O:2][C:3]([C:5]1[C:6]([Cl:13])=[N:7][C:8](Cl)=[CH:9][C:10]=1[CH3:11])=[O:4].C([O-])([O-])=O.[K+].[K+].[NH:20]1[CH2:25][CH2:24][O:23][CH2:22][CH2:21]1.O>CN(C=O)C>[CH3:1][O:2][C:3]([C:5]1[C:6]([Cl:13])=[N:7][C:8]([N:20]2[CH2:25][CH2:24][O:23][CH2:22][CH2:21]2)=[CH:9][C:10]=1[CH3:11])=[O:4]

참가 물질

6

반응물 4

HCID 962WaterHCID 8083MorpholineHCID 11430Potassium CarbonateHCID 46911843Methyl 2,6-dichloro-4-methylnicotinate

생성물 1

HCID 866643312-Chloro-4-methyl-6-morpholino-pyridine-3-carboxylic acid methylester수율 30.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 5.2 g (23.7 mmol) 2,6-dichloro-4-methyl-pyridine-3-carboxylic acid methylester, 3.94 g (28.5 mmol) K2CO3 and 2.06 ml (23.7 mmol) morpholine in DMF (48 ml) was heated to 60° C. for 16 h. Then the mixture was poured into water and extracted with EtOAc. The organic layer was washed with water and brine, dried over Na2SO4 and concentrated in vacuo. Purification of the residue by CC (hexane/EtOAc 4:1) provided 1.95 g (7.2 mmol, 30%) 2-chloro-4-methyl-6-morpholino-pyridine-3-carboxylic acid methylester.

후처리

  1. extractionextracted with EtOAc
  2. washThe organic layer was washed with water and brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated in vacuo
  5. customPurification of the residue by CC (hexane/EtOAc 4:1)

출처 및 근거

ORD 기록
ord-bff0af5adf0848cbbf883efc671b259b
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08552200B2

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