Hydrochloric Acid → Gsk-2245035

HRID 2367967노트

반응식

HRID 2367967 반응식
Cl.[CH3:2][C@H:3]([O:7][C:8]1[N:16]=[C:15]2[C:11]([N:12]=[C:13]([O:28]C)[N:14]2[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][N:22]2[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]2)=[C:10]([NH2:30])[N:9]=1)[CH2:4][CH2:5][CH3:6]>O1CCOCC1.CO>[NH2:30][C:10]1[N:9]=[C:8]([O:7][C@@H:3]([CH3:2])[CH2:4][CH2:5][CH3:6])[N:16]=[C:15]2[C:11]=1[NH:12][C:13](=[O:28])[N:14]2[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][N:22]1[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27]1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 592525742-{[(1S)-1-Methylbutyl]oxy}-8-(methyloxy)-9-[5-(1-piperidinyl)pentyl]-9H-purin-6-amine2회

생성물 1

HCID 44623937Gsk-2245035수율 83.3%

시약·촉매·용매 2

HCID 887Methanol용매3회HCID 312751,4-Dioxane용매

실험 절차

A solution of hydrogen chloride in dioxane (4M, 0.71 mL) was added to a solution of 2-{[(1S)-1-methylbutyl]oxy}-8-(methyloxy)-9-[5-(1-piperidinyl)pentyl]-9H-purin-6-amine (for example, as prepared for Intermediate 9) (0.046 g, 0.126 mmol) in methanol (3 mL). The resultant mixture was allowed to stand overnight at room temperature and then blown down under nitrogen. The residue was dissolved in methanol and loaded onto a 2 g aminopropyl SPE cartridge (pre-conditioned with methanol), eluted with methanol and the resultant solution blown down under nitrogen to give the title compound as a yellow solid (40.97 mg).

후처리

  1. washeluted with methanol

출처 및 근거

ORD 기록
ord-f9fe5cc21ec540ac9a32bda322aa0589
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08703754B2

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