Dimethylformamide → 11-{1-[2-(Phenyl)ethyl]piperidin-4-yl}-5H,11H-pyrrolo[2,1-c][1,4]benzoxazepine oxalate

HRID 2118995노트

반응식

[NH:1]1[CH2:6][CH2:5][CH:4]([CH:7]2[C:13]3=[CH:14][CH:15]=[CH:16][N:12]3[CH2:11][C:10]3[CH:17]=[CH:18][CH:19]=[CH:20][C:9]=3[O:8]2)[CH2:3][CH2:2]1.Br[CH2:22][CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.[C:30]([O-:33])([O-:32])=O.[K+].[K+].CN(C=[O:40])C>>[C:9]([OH:8])(=[O:40])[C:30]([OH:33])=[O:32].[C:24]1([CH2:23][CH2:22][N:1]2[CH2:2][CH2:3][CH:4]([CH:7]3[C:13]4=[CH:14][CH:15]=[CH:16][N:12]4[CH2:11][C:10]4[CH:17]=[CH:18][CH:19]=[CH:20][C:9]=4[O:8]3)[CH2:5][CH2:6]2)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

참가 물질

반응물 4

HCID 6228Dimethylformamide

HCID 7666Phenethyl bromide

HCID 11430Potassium Carbonate

HCID 1368935811-(piperdin-4-yl)-5H,11H-pyrrolo[2,1-c][1,4]benzoxazepine

생성물 1

HCID 2019167911-{1-[2-(Phenyl)ethyl]piperidin-4-yl}-5H,11H-pyrrolo[2,1-c][1,4]benzoxazepine oxalate

반응 조건

온도: 90 °C

실험 절차

To 50 ml DMF were added 11-(piperidin-4-yl)-5H,11H-pyrrolo[2,1-c][1,4]benzoxazepine (4.5 g, 0.017 mole), (2-bromoethyl)benzene (4.3 ml, 0.03 mole), milled K2CO3 (10.0 g, 0.07 mole) and KI (0.01 g). After stirring at 90° C. for four hours the mixture was cooled and filtered, and the filtrate was concentrated in vacuo to an oil. This oil was dissolved in ethyl acetate, washed twice with water and dried (saturated NaCl, anhydrous MgSO4).

후처리

temperaturewas cooled
filtrationfiltered
concentrationthe filtrate was concentrated in vacuo to an oil
dissolutionThis oil was dissolved in ethyl acetate
washwashed twice with water
dry with materialdried (saturated NaCl, anhydrous MgSO4)

출처 및 근거

ORD 기록: ord-f67224a0e8b846118a1d961cef5e9627
출처 데이터셋: uspto-grants-1987_07
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04681879

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