Trimethyl phosphite → Dimethyl (2-chloro-4-morpholinopyrido[3,2-d]pyrimidin-6-yl)methylphosphonate

HRID 2091849ノート

反応式

HRID 2091849 の反応式
Br[CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[N:7]=[C:8]([Cl:19])[N:9]=[C:10]([N:13]3[CH2:18][CH2:17][O:16][CH2:15][CH2:14]3)[C:11]=2[N:12]=1.[P:20]([O:25]C)([O:23][CH3:24])[O:21][CH3:22]>>[Cl:19][C:8]1[N:9]=[C:10]([N:13]2[CH2:18][CH2:17][O:16][CH2:15][CH2:14]2)[C:11]2[N:12]=[C:3]([CH2:2][P:20](=[O:25])([O:23][CH3:24])[O:21][CH3:22])[CH:4]=[CH:5][C:6]=2[N:7]=1

参加物

3

反応物 2

HCID 8472Trimethyl phosphiteHCID 584049784-(6-(Bromomethyl)-2-chloropyrido[3,2-D]pyrimidin-4-YL)morpholine

生成物 1

HCID 58405032Dimethyl (2-chloro-4-morpholinopyrido[3,2-d]pyrimidin-6-yl)methylphosphonate

反応条件

温度
120 °C

実験手順

To 4-(6-(bromomethyl)-2-chloropyrido[3,2-d]pyrimidin-4-yl)morpholine 7 (2 g) was added Trimethyl Phosphite (30 eq) and the reaction was refluxed at 120° C. for 90 minutes. The reaction was cooled and concentrated to dryness under vacuum. To the dried crude was added water, upon which a yellow solid crashed out and was filtered and dried overnight under vacuum to afford 2 g of pure dimethyl (2-chloro-4-morpholinopyrido[3,2-d]pyrimidin-6-yl)methylphosphonate.

後処理

  1. temperatureThe reaction was cooled
  2. concentrationconcentrated to dryness under vacuum
  3. customTo the dried crude
  4. additionwas added water
  5. filtrationwas filtered
  6. customdried overnight under vacuum

出典と根拠

ORDレコード
ord-ddbfaa5bc57845c7b4533a03f540aead
出典データセット
uspto-grants-2013_05
特許番号
US08440651B2

反応ノート

読み込み中…