Water → 151539-47-8

HRID 1081808ノート

反応式

HRID 1081808 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:25]=[CH:26][C:27]=1O)/[CH:5]=[CH:6]/[C:7]1[N:15]([CH3:16])[C:14]2[C:13](=[O:17])[N:12]([CH2:18][CH2:19][CH3:20])[C:11](=[O:21])[N:10]([CH2:22][CH2:23][CH3:24])[C:9]=2[N:8]=1.[CH2:29](I)[CH3:30].[C:32](=[O:35])([O-])[O-].[K+].[K+].O.[CH3:39]N(C)C=O>>[CH2:29]([O:1][C:2]1[CH:3]=[C:4]([CH:25]=[CH:26][C:27]=1[O:35][CH2:32][CH3:39])/[CH:5]=[CH:6]/[C:7]1[N:15]([CH3:16])[C:14]2[C:13](=[O:17])[N:12]([CH2:18][CH2:19][CH3:20])[C:11](=[O:21])[N:10]([CH2:22][CH2:23][CH3:24])[C:9]=2[N:8]=1)[CH3:30]

参加物

6

反応物 5

HCID 962WaterHCID 6228DimethylformamideHCID 6340IodoethaneHCID 11430Potassium Carbonate2 回HCID 135665338(8E)-8-[(2Z)-2-(3-hydroxy-4-oxo-1-cyclohexa-2,5-dienylidene)ethylidene ]-7-methyl-1,3-dipropyl-9H-purine-2,6-dione

生成物 1

HCID 6448800151539-47-8収率 53%

実験手順

Compound 53 (390 mg, 1.01 mmol) obtained in Reference Example 46 was dissolved in 10 ml of dimethylformamide. To the solution were added 0.20 ml (2.50 mmol) of ethyl iodide and 420 mg (3.04 mmol) of potassium carbonate, and the mixture was stirred overnight at room temperature. Water was added thereto to dissolve potassium carbonate and deposited crystals were collected by filtration. The collected crude crystals were recrystallized from hexane/ethyl acetate to give 237 mg (yield 53%) of Compound 54 as pale yellow needles.

後処理

  1. filtrationwere collected by filtration
  2. customThe collected crude crystals
  3. customwere recrystallized from hexane/ethyl acetate

出典と根拠

ORDレコード
ord-785c61d472b54499985a802eb5337699
出典データセット
uspto-grants-1996_12
特許番号
US05587378

反応ノート

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