5-Chloro-2-furaldehyde → HCID 76285306、化合物

HRID 624556

反応式

HRID 624556 の反応式
[NH2:1][CH2:2][CH2:3][N:4]1[C:12]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[CH:14]=2)=[C:11]2[C:6]([N:7]([CH3:23])[C:8](=[O:22])[N:9]([CH3:21])[C:10]2=[O:20])=[CH:5]1.[Cl:24][C:25]1[O:29][C:28]([CH:30]=O)=[CH:27][CH:26]=1>C(O)C.C(O)(C(F)(F)F)=O>[Cl:24][C:25]1[O:29][C:28]([CH:30]2[C:5]3=[C:6]4[C:11](=[C:12]([C:13]5[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[CH:14]=5)[N:4]3[CH2:3][CH2:2][NH:1]2)[C:10](=[O:20])[N:9]([CH3:21])[C:8](=[O:22])[N:7]4[CH3:23])=[CH:27][CH:26]=1

参加物

5

反応物 2

HCID 27696305-Chloro-2-furaldehydeHCID 86722880HCID 86722880、化合物2 回

生成物 1

HCID 76285306HCID 76285306、化合物

試薬・触媒・溶媒 2

HCID 6422Trifluoroacetic acid触媒HCID 702Ethanol溶媒2 回

反応条件

温度
50 °C

実験手順

6-(2-Amino-ethyl)-5-(3-chloro-phenyl)-1,3-dimethyl-1,6-dihydro-pyrrolo[3,4-d]pyrimidine-2,4-dione (Intermediate B) (150 mg, 0.451 mmol) and 5-chlorofuran-2-carbaldehyde (commercially available, 58.8 mg, 0.451 mmol) were suspended in ethanol (1.2 ml). The mixture was heated at 50° C. under microwave irradiation for 1 hour. TFA (4 drops) was added to the reaction mixture and heating continued at 60° C. for a further 30 mins under microwave irradiation. The reaction mixture was diluted with ethanol (0.5 mL) and purified using mass directed HPLC. The product containing fractions were combined and evaporated under reduced pressure to afford a white solid which was dried under vacuum at 50° C. for 16 h to afford the title compound as a pale tan solid;

後処理

  1. temperatureheating
  2. customcontinued at 60° C. for a further 30 mins under microwave irradiation
  3. custompurified
  4. additionThe product containing fractions
  5. customevaporated under reduced pressure
  6. customto afford a white solid which
  7. customwas dried under vacuum at 50° C. for 16 h

出典と根拠

ORDレコード
ord-5a51311e7c1f464badbed1b4e2494218
出典データセット
uspto-grants-2016_04
特許番号
US09303035B2

関連ノート

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