Urea → 6-(2,4-Difluoro-phenoxy)-1H-pyrido[3,4-d]pyrimidine-2,4-dione

HRID 457702ノート

反応式

HRID 457702 の反応式
CO[C:3](=[O:20])[C:4]1[C:9]([NH2:10])=[CH:8][N:7]=[C:6]([O:11][C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][C:13]=2[F:19])[CH:5]=1.[NH2:21][C:22](N)=[O:23]>O>[F:19][C:13]1[CH:14]=[C:15]([F:18])[CH:16]=[CH:17][C:12]=1[O:11][C:6]1[N:7]=[CH:8][C:9]2[NH:10][C:22](=[O:23])[NH:21][C:3](=[O:20])[C:4]=2[CH:5]=1

参加物

4

反応物 2

HCID 1176UreaHCID 588201935-Amino-2-(2,4-difluoro-phenoxy)-isonicotinic acid methyl ester

生成物 1

HCID 184406256-(2,4-Difluoro-phenoxy)-1H-pyrido[3,4-d]pyrimidine-2,4-dione収率 98.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Compound (1C) (4.2 g, 15.0 mmol) and urea (9.0 g, 10 eq) were heated to a melt at 160° C. with stirring. After 2 hours, the melt solidified and by TLC the reaction was complete. The reaction mixture was cooled to room temperature, water (250 mL) was added, and the resulting mixture was left to stand for 1 hour. Then the solids were broken up with a spatula and the mixture was stirred vigorously for 1 hour. After suction filtration, a tan powder was collected which was air-dried in the frit for two days. Drying under high vacuum at 56° C. gave the title compound (1D) as a tan powder (4.307 g, (M−H)−=290, M.P.>300° C.).

後処理

  1. waitthe resulting mixture was left
  2. waitto stand for 1 hour
  3. stirringthe mixture was stirred vigorously for 1 hour
  4. filtrationAfter suction filtration
  5. customa tan powder was collected which
  6. customwas air-dried in the frit for two days
  7. customDrying under high vacuum at 56° C.

出典と根拠

ORDレコード
ord-b22efac00e8b497f82147eca830e8a3b
出典データセット
uspto-grants-2007_03
特許番号
US07189731B2

反応ノート

読み込み中…