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

HRID 1043576노트

반응식

HRID 1043576 반응식
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

참가 물질

3

반응물 2

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

생성물 1

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

반응 조건

온도
120 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-27097a99895242a391a6c636b5f3094d
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08563540B2

반응 노트

불러오는 중…