Water → Acetic acid, (4-(2-(1,3-diethyl-2,3,6,7-tetrahydro-7-methyl-2,6-dioxo- 1H-purin-8-yl)ethenyl)phenoxy)-, ethyl ester, (E)-

HRID 1081850노트

반응식

HRID 1081850 반응식
[CH2:1]([N:3]1[C:12](=[O:13])[C:11]2[N:10]([CH3:14])[C:9](/[CH:15]=[CH:16]/[C:17]3[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=3)=[N:8][C:7]=2[N:6]([CH2:24][CH3:25])[C:4]1=[O:5])[CH3:2].C(=O)([O-])[O-].[K+].[K+].Cl[CH2:33][C:34]([O:36][CH2:37][CH3:38])=[O:35].O>CN(C)C=O>[CH2:37]([O:36][C:34]([CH2:33][O:23][C:20]1[CH:19]=[CH:18][C:17](/[CH:16]=[CH:15]/[C:9]2[N:10]([CH3:14])[C:11]3[C:12](=[O:13])[N:3]([CH2:1][CH3:2])[C:4](=[O:5])[N:6]([CH2:24][CH3:25])[C:7]=3[N:8]=2)=[CH:22][CH:21]=1)=[O:35])[CH3:38]

참가 물질

6

반응물 4

HCID 962WaterHCID 7751Ethyl chloroacetateHCID 11430Potassium Carbonate2회HCID 1356653431H-Purine-2,6-dione, 3,7-dihydro-1,3-diethyl-8-(2-(4-hydroxyphenyl)eth enyl)-7-methyl-, (E)-

생성물 1

HCID 6448954Acetic acid, (4-(2-(1,3-diethyl-2,3,6,7-tetrahydro-7-methyl-2,6-dioxo- 1H-purin-8-yl)ethenyl)phenoxy)-, ethyl ester, (E)-수율 91%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Compound 175 (300 mg, 0.88 mmol) obtained in Reference Example 114 was dissolved in 10 ml of dimethyl formamide. To the solution were added 731 mg (5.29 mmol) of potassium carbonate and 0.47 ml (4.41 mmol) of ethyl chloroacetate, and the mixture was stirred at room temperature for 2 hours. Water was added thereto to dissolve potassium carbonate and the deposited crystals were collected by filtration. The collected crude crystals were dissolved in chloroform, washed with a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate, followed by evaporation under reduced pressure. The residue was recrystallized from hexane/ethyl acetate to give 341 mg (yield 91%) of Compound 180 as pale yellow needles.

후처리

  1. filtrationthe deposited crystals were collected by filtration
  2. customThe collected crude crystals
  3. dissolutionwere dissolved in chloroform
  4. washwashed with a saturated aqueous solution of sodium chloride
  5. dry with materialdried over anhydrous sodium sulfate
  6. customfollowed by evaporation under reduced pressure
  7. customThe residue was recrystallized from hexane/ethyl acetate

출처 및 근거

ORD 기록
ord-d2fa3b9946424d6da84d3ff4bed8c21a
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05587378

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