Carbamimidic acid, methyl ester, sulfate (1:1) → 4'-[(2-Methoxy-6-oxo-4-propyl-1,6-dihydropyrimidin-5-yl)methyl]biphenyl-2-carbonitrile

HRID 1718241노트

반응식

HRID 1718241 반응식
S(O)(O)(=O)=O.[C:6](=[NH:10])([O:8][CH3:9])[NH2:7].C[O-].[Na+].[C:14]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[C:22]1[CH:27]=[CH:26][C:25]([CH2:28][CH:29]([C:35](=O)[CH2:36][CH2:37][CH3:38])[C:30](OCC)=[O:31])=[CH:24][CH:23]=1)#[N:15]>CO>[CH3:9][O:8][C:6]1[NH:7][C:30](=[O:31])[C:29]([CH2:28][C:25]2[CH:26]=[CH:27][C:22]([C:17]3[C:16]([C:14]#[N:15])=[CH:21][CH:20]=[CH:19][CH:18]=3)=[CH:23][CH:24]=2)=[C:35]([CH2:36][CH2:37][CH3:38])[N:10]=1

참가 물질

5

반응물 3

HCID 169039Carbamimidic acid, methyl ester, sulfate (1:1)HCID 10020734Ethyl 2-[(2'-cyanobiphenyl-4-yl)methyl]-3-oxohexanoateHCID 10942334Sodium Methoxide

생성물 1

HCID 1360267204'-[(2-Methoxy-6-oxo-4-propyl-1,6-dihydropyrimidin-5-yl)methyl]biphenyl-2-carbonitrile수율 16.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of methyl imidocarbamate sulfate (10 g), 28% sodium methoxide (26 mL) and ethyl 2-[(2′-cyanobiphenyl-4-yl)methyl]-3-oxohexanoate (15.8 g) in methanol (100 mL) was stirred overnight at room temperature. The solvent was evaporated under reduced pressure, and water and acetic acid were added. The precipitated solid was collected by filtration, washed with water and diethyl ether to give the title compound (2.62 g, 16%) as a colorless solid.

후처리

  1. customThe solvent was evaporated under reduced pressure, and water and acetic acid
  2. additionwere added
  3. filtrationThe precipitated solid was collected by filtration
  4. washwashed with water and diethyl ether

출처 및 근거

ORD 기록
ord-7c690fa062bb4221902b4ae712358eeb
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07803940B2

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