Hydrochloric Acid → HCID 11994283, 화합물

HRID 1793809노트

반응식

HRID 1793809 반응식
Cl.[NH2:2][C:3]1[C:4](=[O:14])[NH:5][C:6](=[O:13])[N:7]([CH2:10][CH2:11][CH3:12])[C:8]=1[NH2:9].[OH:15][C:16]12[CH2:23][CH2:22][C:19]([C:24](O)=O)([CH2:20][CH2:21]1)[CH2:18][CH2:17]2.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(CC)CC.O.[OH-].[Na+].Cl>CN(C=O)C>[OH:15][C:16]12[CH2:23][CH2:22][C:19]([C:24]3[NH:2][C:3]4[C:4](=[O:14])[NH:5][C:6](=[O:13])[N:7]([CH2:10][CH2:11][CH3:12])[C:8]=4[N:9]=3)([CH2:20][CH2:21]1)[CH2:18][CH2:17]2

참가 물질

9

반응물 7

HCID 313Hydrochloric AcidHCID 962WaterHCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 11994282HCID 11994282, 화합물HCID 125601364-Hydroxybicyclo[2.2.2]octane-1-carboxylic acid

생성물 1

HCID 11994283HCID 11994283, 화합물수율 38.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

5,6-Diamino-1-propyl-1H-pyrimidine-2,4-dione hydrochloride salt (3.4 g) was dissolved in 80 mL of DMF along with 4-hydroxy-bicyclo[2.2.2]octane-1-carboxylic acid (2.5 g, 15 mmol). HATU (5.9 g, 1.05 eq) was added, followed by Et3N (8.30 mL, 4.05 eq). The resulting reaction mixture was stirred at rt overnight. The reaction mixture was filtered to remove some of the precipitate. The filtrate was concentrated under reduced pressure. The resulting residue was dissolved in 60 mL of H2O containing 10 eq of NaOH (5.9 g). The reaction mixture was stirred under reflux for 1 h, cooled to rt and acidified to pH2 with concentrated HCl. The resulting precipitate was collected by filtration and dried to afford 1.85 g of the xanthine derivative.

후처리

  1. customThe resulting reaction mixture
  2. filtrationThe reaction mixture was filtered
  3. customto remove some of the precipitate
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. stirringThe reaction mixture was stirred
  6. temperatureunder reflux for 1 h
  7. temperaturecooled to rt
  8. filtrationThe resulting precipitate was collected by filtration
  9. customdried

출처 및 근거

ORD 기록
ord-1db5e2e77dc84a64b70ece3365399ba4
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07022686B2

반응 노트

불러오는 중…