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

HRID 1673569ノート

反応式

HRID 1673569 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7a78720eb6f14d0a884149fdb28726b6
出典データセット
uspto-grants-2011_08
特許番号
US07998968B2

反応ノート

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