1-Butanol → HCID 11294944、化合物

HRID 411290ノート

反応式

HRID 411290 の反応式
Cl[C:2]1[N:11]=[C:10]([NH2:12])[C:9]2[C:4](=[CH:5][C:6](C)=[C:7](C)[CH:8]=2)[N:3]=1.[CH2:15]([N:22]1[CH2:27][CH2:26][C:25]([CH2:34][NH:35][CH3:36])([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[CH2:24][CH2:23]1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.[C:37](=[O:40])([O-])[O-].[K+].[K+].[CH2:43]([OH:47])CCC>>[CH2:15]([N:22]1[CH2:23][CH2:24][C:25]([CH2:34][N:35]([CH3:36])[C:2]2[N:11]=[C:10]([NH2:12])[C:9]3[C:4](=[CH:5][C:6]([O:40][CH3:37])=[C:7]([O:47][CH3:43])[CH:8]=3)[N:3]=2)([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[CH2:26][CH2:27]1)[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1

参加物

5

反応物 4

HCID 2631-ButanolHCID 11430Potassium CarbonateHCID 11426409HCID 11426409、化合物HCID 185407744-Amino-2-chloro-6,7-dimethylquinazoline

生成物 1

HCID 11294944HCID 11294944、化合物

実験手順

A mixture of 2-chloro-6,7-dimethyl-quinazolin-4-ylamine 1 (X=Cl) (900 mg), (1-benzyl-4-phenyl-piperidin-4-ylmethyl)-methyl-amine 2a (R1=CH3 and R2=phenyl) (440 mg) and potassium carbonate (250 mg) in 1-butanol (20 ml) was refluxed for 18 hours. The cooled reaction mixture was filtered, the filtrate was evaporated, and the residue was distributed between water and dichloromethane. The organic phase was dried over potassium carbonate, filtered, and evaporated. The residue was purified by flash chromatography on silica gel to provide 1.3 g of N2-(1-Benzyl-4-phenyl-piperidin-4-ylmethyl)-6,7-dimethoxy-N2-methyl-quinazoline-2,4-diamine 10, as an oil, MS: 485 (M+).

後処理

  1. customThe cooled reaction mixture
  2. filtrationwas filtered
  3. customthe filtrate was evaporated
  4. dry with materialThe organic phase was dried over potassium carbonate
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was purified by flash chromatography on silica gel

出典と根拠

ORDレコード
ord-bf6a08d9250a42e684b2ac02f805af77
出典データセット
uspto-grants-2003_05
特許番号
US06559153B2

反応ノート

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