4-Methylmorpholine → HCID 44633631, 화합물

HRID 1643427노트

반응식

HRID 1643427 반응식
CN1CCOCC1.[CH3:8][C:9]1[C:17]([OH:18])=[C:16]2[C:12]([CH:13]([C:19]3[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=3)[O:14][CH2:15]2)=[CH:11][N:10]=1.[N+:26]([O:29][CH2:30][CH2:31][CH2:32][C:33](O)=[O:34])([O-:28])=[O:27].Cl.C(N=C=NCCCN(C)C)C>CN(C)C1C=CN=CC=1.ClCCl>[N+:26]([O:29][CH2:30][CH2:31][CH2:32][C:33]([O:18][C:17]1[C:16]2[CH2:15][O:14][C@H:13]([C:19]3[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=3)[C:12]=2[CH:11]=[N:10][C:9]=1[CH3:8])=[O:34])([O-:28])=[O:27]

참가 물질

7

반응물 4

HCID 79724-MethylmorpholineHCID 54910CicletanineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 98340014-(Nitrooxy)butanoic acid

생성물 1

HCID 44633631HCID 44633631, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

N-Methylmorpholine (90 μL, 0.82 mmol) was added to a stirred solution of (R)-(−)-cicletanine (48 mg, 0.18 mmol), 4-(nitrooxy)butanoic acid (27 mg, 0.18 mmol), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (42 mg, 0.22 mmol), and 4-dimethylaminopyridine (9 mg, 0.07 mmol) in dichloromethane (1.8 mL). The solution was stirred overnight at room temperature. The mixture was concentrated under reduced pressure. The residue was purified by HPLC reverse phase (C-18) cluting with acetonitrile/water with 0.05% TFA to afford the title compound as a colorless oil. LC-MS: m/z 392.9 (M+H).

후처리

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customThe residue was purified by HPLC reverse phase (C-18)

출처 및 근거

ORD 기록
ord-36232f41279745a385394f36b82bb15e
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08119806B2

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