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Hydrochloric Acid → HCID 11638190, 화합물

HRID 1835732
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HRID 1835732 반응식
C(OC[N:5]1[C:13]2[C:12](=[O:14])[N:11]([CH2:15][CH2:16][CH2:17][CH2:18][C@H:19]([OH:21])[CH3:20])[C:10](=[O:22])[N:9]([CH3:23])[C:8]=2[N:7]=[C:6]1[S:24][CH3:25])C.Cl>C(O)C>[OH:21][C@H:19]([CH3:20])[CH2:18][CH2:17][CH2:16][CH2:15][N:11]1[C:12](=[O:14])[C:13]2[NH:5][C:6]([S:24][CH3:25])=[N:7][C:8]=2[N:9]([CH3:23])[C:10]1=[O:22]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 54139417HCID 54139417, 화합물

생성물 1

HCID 11638190HCID 11638190, 화합물수율 71.1%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
80 °C

실험 절차

To a solution of (R)-7-ethoxymethyl-1-(5-hydroxyhexyl)-3-methyl-8-methylsulfanylxanthine (20 mg, 0.054 mmol) in ethanol (1.9 ml) was added concentrated hydrochloric acid (0.10 ml). The reaction mixture was stirred at 80° C. for 24 hours. After evaporation of the solvent under reduced pressure, the crude product was purified by flash chromatography on silica gel eluting with ethyl acetate-methanol (7:1) to provide (R)-1-(5-hydroxyhexyl)-3-methyl-8-methylsulfanylxanthine (12 mg, 70% yield) as a white solid.

후처리

  1. customAfter evaporation of the solvent under reduced pressure
  2. customthe crude product was purified by flash chromatography on silica gel eluting with ethyl acetate-methanol (7:1)

출처 및 근거

ORD 기록
ord-4a133af113c94778850a78ff43f4f4a4
출처 데이터셋
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06774130B2

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