2-Pyridinemethanamine → 2-aminopyrido[2,3-d]pyrimidin-7(8H)-one 34

HRID 3189

反応式

HRID 3189 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:20](=[O:21])[N:19]([CH3:22])[C:12]2[N:13]=[C:14](SC)[N:15]=[CH:16][C:11]=2[CH:10]=1.[NH2:23][CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][N:26]=1>CN(C)C=O>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:20](=[O:21])[N:19]([CH3:22])[C:12]2[N:13]=[C:14]([NH:23][CH2:24][C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][N:26]=3)[N:15]=[CH:16][C:11]=2[CH:10]=1

参加物

4

反応物 2

HCID 195092-PyridinemethanamineHCID 107367016-(2,6-Dichlorophenyl)-8-methyl-2-(methylthio)pyrido[2,3-d]pyrimidin-7(8H)-one

生成物 1

HCID 53278812-aminopyrido[2,3-d]pyrimidin-7(8H)-one 34収率 38.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
130 °C

実験手順

A mixture of 0.165 g (0.47 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 37, 1.08 g (10.0 mmol) of 2-(aminomethyl)pyridine and 0.5 mL of dimethylformamide was heated with stirring in a 130° C. oil bath. After 2 minutes, solution was complete. After 2 hours, the excess amine and dimethylformamide were evaporated at reduced pressure. Ether (5 mL) was added to the residue. Crystals immediately developed. Water (5 mL) was added, and the entire mixture was filtered. The cake was washed 5 mL of ether, 5 mL of water, and then dried; wt 0.164 g. Recrystallization from ethyl acetate gave 0.075 g of pure product; mp 198°-201° C.

後処理

  1. temperaturewas heated
  2. waitAfter 2 hours
  3. customthe excess amine and dimethylformamide were evaporated at reduced pressure
  4. additionEther (5 mL) was added to the residue
  5. additionWater (5 mL) was added
  6. filtrationthe entire mixture was filtered
  7. washThe cake was washed 5 mL of ether, 5 mL of water
  8. customdried
  9. customRecrystallization from ethyl acetate

出典と根拠

ORDレコード
ord-4065ebd450dd42b9b396a7e3dbade98c
出典データセット
uspto-grants-1998_03
特許番号
US05733914

関連ノート

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