Morpholine → 1-[5-(3-Cyclobutyl-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yloxy)-pyrazin-2-yl]-1-morpholin-4-yl-methanone

HRID 222693노트

반응식

HRID 222693 반응식
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[CH:7]1([N:11]2[CH2:17][CH2:16][C:15]3[CH:18]=[C:19]([O:22][C:23]4[N:24]=[CH:25][C:26]([C:29](Cl)=[O:30])=[N:27][CH:28]=4)[CH:20]=[CH:21][C:14]=3[CH2:13][CH2:12]2)[CH2:10][CH2:9][CH2:8]1.CCN(CC1C=CC=CC=1)CC.C=CC1C=CC=CC=1.C=CC1C=CC(C=C)=CC=1>ClCCl>[CH:7]1([N:11]2[CH2:17][CH2:16][C:15]3[CH:18]=[C:19]([O:22][C:23]4[N:24]=[CH:25][C:26]([C:29]([N:1]5[CH2:6][CH2:5][O:4][CH2:3][CH2:2]5)=[O:30])=[N:27][CH:28]=4)[CH:20]=[CH:21][C:14]=3[CH2:13][CH2:12]2)[CH2:8][CH2:9][CH2:10]1

참가 물질

5

반응물 3

HCID 8083MorpholineHCID 16212021N-benzyl-N-ethylethanamine;1,4-bis(ethenyl)benzene;styreneHCID 866032205-(3-Cyclobutyl-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yloxy)-pyrazine-2-carbonyl chloride

생성물 1

HCID 104091851-[5-(3-Cyclobutyl-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yloxy)-pyrazin-2-yl]-1-morpholin-4-yl-methanone

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Morpholine (0.17 ml, 2.0 mmol) was added to a stirred solution of the product of step 1 (394 mg, 1 mmol) and diethylaminomethyl polystyrene (1.88 g, 3.2 mmol/g, 6 mmol) in dichloromethane (10 ml). The resulting mixture was allowed to stir at room temperature for 24 hours and the filtered. The filtrate was concentrated in vacuo and the resulting crude residue was purified column chromatography eluting with a mixture of 0.880 ammonia:ethanol:dichloromethane (1:9:90) to afford the title compound (E123). MS (ES+) m/e 409 [M+H]+.

후처리

  1. concentrationThe filtrate was concentrated in vacuo
  2. customthe resulting crude residue was purified column chromatography
  3. washeluting with a mixture of 0.880 ammonia:ethanol:dichloromethane (1:9:90)

출처 및 근거

ORD 기록
ord-6c467f3483014120a1605e9858a8af69
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08207331B2

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