1,3-Benzodioxol-5-amine → 2-(Benzo[1,3]dioxol-5-ylamino)-6-(2,6-dichlorophenyl)-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one

HRID 3195

反応式

HRID 3195 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:22](=[O:23])[N:21]([CH3:24])[C:12]2[N:13]=[C:14](S(C)(=O)=O)[N:15]=[CH:16][C:11]=2[CH:10]=1.[CH2:25]1[O:34][C:33]2[CH:32]=[CH:31][C:29]([NH2:30])=[CH:28][C:27]=2[O:26]1>C(OCC)(=O)C>[O:34]1[C:33]2[CH:32]=[CH:31][C:29]([NH:30][C:14]3[N:15]=[CH:16][C:11]4[CH:10]=[C:9]([C:3]5[C:2]([Cl:1])=[CH:7][CH:6]=[CH:5][C:4]=5[Cl:8])[C:22](=[O:23])[N:21]([CH3:24])[C:12]=4[N:13]=3)=[CH:28][C:27]=2[O:26][CH2:25]1

参加物

4

反応物 2

HCID 843101,3-Benzodioxol-5-amineHCID 105961576-(2,6-Dichlorophenyl)-8-methyl-2-methylsulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one

生成物 1

HCID 116046182-(Benzo[1,3]dioxol-5-ylamino)-6-(2,6-dichlorophenyl)-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
200 °C

実験手順

A mixture of 0.113 g (0.29 mmol) of 6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 39 and 0.50 g (3.70 mmol) of 3,4-methylenedioxyaniline was heated, with stirring, in a 200° C. oil bath. The resulting solution was heated for 5 minutes and cooled to room temperature. Ethyl acetate (2 mL) was added, and some traces of solids were filtered. The crystals that slowly developed in the filtrate were filtered and washed with 2 mL of ethyl acetate; wt 0.080 g. The solid was purified to remove dark colors by silica gel chromatography, eluting with chloroform and then 50% hexane/ethyl acetate to obtain pure crystalline product; wt 0.054 g; mp 240°-241° C.

後処理

  1. temperaturewas heated
  2. temperatureThe resulting solution was heated for 5 minutes
  3. temperaturecooled to room temperature
  4. filtrationsome traces of solids were filtered
  5. filtrationwere filtered
  6. washwashed with 2 mL of ethyl acetate
  7. customThe solid was purified
  8. customto remove dark colors by silica gel chromatography
  9. washeluting with chloroform
  10. custom50% hexane/ethyl acetate to obtain pure crystalline product

出典と根拠

ORDレコード
ord-229e6ead42474df5b581ec87f76dc9f1
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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