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Hydrochloric Acid → 2-(Butyloxy)-9-(4-piperidinylmethyl)-9H-purin-6-amine hydrochloride

HRID 1044948
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반응식

HRID 1044948 반응식
[ClH:1].[NH2:2][C:3]1[N:11]=[C:10]([O:12][CH2:13][CH2:14][CH2:15][CH3:16])[N:9]=[C:8]2[C:4]=1[N:5]=[C:6](OC)[N:7]2[CH2:17][CH:18]1[CH2:23][CH2:22][N:21](C(OC(C)(C)C)=O)[CH2:20][CH2:19]1>O1CCOCC1.CO>[ClH:1].[CH2:13]([O:12][C:10]1[N:9]=[C:8]2[C:4]([N:5]=[CH:6][N:7]2[CH2:17][CH:18]2[CH2:19][CH2:20][NH:21][CH2:22][CH2:23]2)=[C:3]([NH2:2])[N:11]=1)[CH2:14][CH2:15][CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 583060912-Butoxy-9-(1-tert-butoxycarbonylpiperidin-4-ylmethyl)-8-methoxyadenine

생성물 1

HCID 671801992-(Butyloxy)-9-(4-piperidinylmethyl)-9H-purin-6-amine hydrochloride

시약·촉매·용매 2

HCID 887Methanol용매HCID 312751,4-Dioxane용매

실험 절차

4N hydrogen chloride in dioxane (5.3 mL) was added to a solution of 1,1-dimethylethyl 4-{[6-amino-2-(butyloxy)-8-(methyloxy)-9H-purin-9-yl]methyl}-1-piperidinecarboxylate (630 mg) in methanol (16 mL). After 4.5 hours at room temperature, the reaction mixture was concentrated and dried under high vacuum. Purification by chromatography on silica gel eluting with a gradient of chloroform/methanol/water 90:10:1 to 75:25:1 afforded the title compound as a white solid (404 mg).

후처리

  1. concentrationthe reaction mixture was concentrated
  2. customdried under high vacuum
  3. customPurification by chromatography on silica gel eluting with a gradient of chloroform/methanol/water 90:10:1 to 75:25:1

출처 및 근거

ORD 기록
ord-4e2bf0b0aa2a49478465fe2449809df0
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08563717B2

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