Hydrochloric Acid → Gsk-2245035

HRID 590498ノート

反応式

HRID 590498 の反応式
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

参加物

5

反応物 2

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

生成物 1

HCID 44623937Gsk-2245035収率 83.3%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒3 回HCID 312751,4-Dioxane溶媒

実験手順

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 (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).

後処理

  1. washeluted with methanol

出典と根拠

ORDレコード
ord-3143ce38deb44679a6648301cf6b0f2f
出典データセット
uspto-grants-2016_01
特許番号
US09233962B2

反応ノート

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