Morpholine → (6-Aminopyridin-3-yl)(morpholino)methanone

HRID 68457

반응식

HRID 68457 반응식
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.Cl.CN(C)CCCN=C=NCC.ON1C2C=CC=CC=2N=N1.[NH2:29][C:30]1[CH:38]=[CH:37][C:33]([C:34](O)=[O:35])=[CH:32][N:31]=1>C(O)C>[NH2:29][C:30]1[N:31]=[CH:32][C:33]([C:34]([N:1]2[CH2:6][CH2:5][O:4][CH2:3][CH2:2]2)=[O:35])=[CH:37][CH:38]=1

참가 물질

6

반응물 4

HCID 8083MorpholineHCID 184966-Aminonicotinic acidHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

생성물 1

HCID 59259223(6-Aminopyridin-3-yl)(morpholino)methanone수율 34.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of morpholine (9.00 g, 103 mmol) in 400 mL ethanol was added N-(3-Dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (10.0 g, 52.2 mmol), 1-hydroxybenzotriazole (7.00 g, 51.8 mmol), and 6-aminonicotinic acid (6.00 g, 43.4 mmol). After stirring for 18 hours, the resulting solid was filtered. This was triturated with a mixture of 100 mL methanol and 100 mL dichloromethane to yield (6-Amino-pyridin-3-yl)-morpholin-4-yl-methanone (3.08 g, 14.9 mmol). MS (ESI) 208.1 (M+H)+.

후처리

  1. filtrationthe resulting solid was filtered
  2. customThis was triturated with a mixture of 100 mL methanol and 100 mL dichloromethane

출처 및 근거

ORD 기록
ord-333f6a181a9a4c4b8df2a3415efa8db1
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822457B2

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