Water → 151539-47-8

HRID 1077469ノート

反応式

HRID 1077469 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 54 (390 mg, 1.01 mmol) obtained in Reference Example 51 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 55 as pale yellow needles.

後処理

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

出典と根拠

ORDレコード
ord-8aed19cc2b054584999af02a63b7ffe3
出典データセット
uspto-grants-1996_08
特許番号
US05543415

反応ノート

読み込み中…