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

HRID 1043576ノート

反応式

HRID 1043576 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-27097a99895242a391a6c636b5f3094d
出典データセット
uspto-grants-2013_10
特許番号
US08563540B2

反応ノート

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