Hydrochloric Acid → HCID 60123474, 화합물

HRID 2416424노트

반응식

HRID 2416424 반응식
Cl.C([O:5][C@H:6]([CH3:33])[CH2:7][CH2:8][CH2:9][CH2:10][N:11]1[C:16](=[O:17])[C:15]2[C:18](=[O:30])[CH:19]=[C:20]([CH3:29])[N:21]([CH2:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[C:14]=2[N:13]([CH3:31])[C:12]1=[O:32])(=O)C>CO>[CH2:22]([N:21]1[C:14]2[N:13]([CH3:31])[C:12](=[O:32])[N:11]([CH2:10][CH2:9][CH2:8][CH2:7][C@H:6]([OH:5])[CH3:33])[C:16](=[O:17])[C:15]=2[C:18](=[O:30])[CH:19]=[C:20]1[CH3:29])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 69733083HCID 69733083, 화합물

생성물 1

HCID 60123474HCID 60123474, 화합물수율 60%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

37% Aqueous hydrochloric acid (5 ml) was added to a solution of the crude (R)-3-(5-acetoxyhexyl)-8-benzyl-1,7-dimethylpyrido[2,3-d]pyrimidine-2,4,5(1H,3H,8H)-trione in methanol (20 ml). After stirring at room temperature for 18 hours, the solution was concentrated under reduced pressure. The residue was treated with water (20 ml) and extracted with ethyl acetate (2×20 ml). The combined extracts were concentrated under reduced pressure to provide an oil which solidified on standing. The solid was recrystallized (ethyl acetate-hexanes) to afford (R)-8-Benzyl-1,7-dimethyl-3-(5-hydroxyhexyl)pyrido[2,3-d]pyrimidine-2,4,5(1H,3H,8H)-trione (1.26 g, 60% yield for 2 steps) as a white powder. 1H NMR (300 MHz, CDCl3) δ 1.19 (d, 3H), 1.35-1.52 (m, 4H), 1.54-1.70 (m, 2H), 2.47 (s,3H), 3.63 (s, 3H), 3.78 (m, 1H), 4.05 (t, 2H), 5.29 (s, 2H), 6.54 (s, 1H), 7.25-7.55 (m, 5H).

후처리

  1. concentrationthe solution was concentrated under reduced pressure
  2. additionThe residue was treated with water (20 ml)
  3. extractionextracted with ethyl acetate (2×20 ml)
  4. concentrationThe combined extracts were concentrated under reduced pressure
  5. customto provide an oil which
  6. customThe solid was recrystallized (ethyl acetate-hexanes)

출처 및 근거

ORD 기록
ord-4e475390b6f54f08b80c3f2ce666bfdb
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06825180B2

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