Dimethyl Sulfate → 1H-Purine-2,6-dione, 3,7-dihydro-8-(2-(1,1'-biphenyl)-4-ylethenyl)-1,3-diethyl-7-methyl-, (E)-

HRID 375364

반응식

HRID 375364 반응식
[CH2:1]([N:3]1[C:12](=[O:13])[C:11]2[NH:10][C:9](/[CH:14]=[CH:15]/[C:16]3[CH:21]=[CH:20][C:19]([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)=[CH:18][CH:17]=3)=[N:8][C:7]=2[N:6]([CH2:28][CH3:29])[C:4]1=[O:5])[CH3:2].[OH-].[Na+].S(OC)(O[CH3:36])(=O)=O>O.CO>[CH2:1]([N:3]1[C:12](=[O:13])[C:11]2[N:10]([CH3:36])[C:9](/[CH:14]=[CH:15]/[C:16]3[CH:21]=[CH:20][C:19]([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)=[CH:18][CH:17]=3)=[N:8][C:7]=2[N:6]([CH2:28][CH3:29])[C:4]1=[O:5])[CH3:2]

참가 물질

6

반응물 3

HCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 64489391H-Purine-2,6-dione, 3,7-dihydro-8-(2-(1,1'-biphenyl)-4-ylethenyl)-1,3-diethyl-, (E)-

생성물 1

HCID 64489401H-Purine-2,6-dione, 3,7-dihydro-8-(2-(1,1'-biphenyl)-4-ylethenyl)-1,3-diethyl-7-methyl-, (E)-수율 30.8%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

실험 절차

Compound 163 (1.50 g, 3.89 mmol) obtained in Reference Example 104 was suspended in a mixed solvent of 13 ml of water, 3.9 ml of a 2N aqueous solution of sodium hydroxide, and 7 ml of methanol. To the suspension was dropwise added 0.55 ml (5.83 mmol) of dimethyl sulfate, and the resultant mixture was stirred at 60° C.; for 4 hours. Water (10 ml) was added thereto, and the deposited crystals were collected by filtration and dried. The obtained crude crystals were purified by silica gel column chromatography, followed by recrystallization from ethyl acetate to give 480 mg (yield 28%) of Compound 164 as yellow columns.

후처리

  1. filtrationthe deposited crystals were collected by filtration
  2. customdried
  3. customThe obtained crude crystals
  4. customwere purified by silica gel column chromatography
  5. customfollowed by recrystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-443fd262b8e94838847f9dc1018d83ea
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05484920

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