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Water → HCID 9925691、化合物

HRID 1602877
ノート
印刷プレビュー

反応式

HRID 1602877 の反応式
[H-].[Na+].[OH:3][CH2:4][C:5]1[CH:10]=[CH:9][N:8]=[CH:7][CH:6]=1.[CH2:11]([C:15]1[CH:20]=[C:19](Cl)[N:18]2[N:22]=[CH:23][CH:24]=[C:17]2[N:16]=1)[CH2:12][CH:13]=[CH2:14].O>CN(C=O)C>[CH2:11]([C:15]1[CH:20]=[C:19]([O:3][CH2:4][C:5]2[CH:10]=[CH:9][N:8]=[CH:7][CH:6]=2)[N:18]2[N:22]=[CH:23][CH:24]=[C:17]2[N:16]=1)[CH2:12][CH:13]=[CH2:14]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 114724-HydroxymethylpyridineHCID 24758Sodium hydrideHCID 15462308HCID 15462308、化合物

生成物 1

HCID 9925691HCID 9925691、化合物収率 42.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
0 °C

実験手順

60% sodium hydride, 0.55 g, was added to a 10 ml-solution of 1.6 g of 4-(hydroxymethyl)pyridine in DMF while being ice-cooled. After the mixture was stirred at 0° C. for 30 minutes, a DMF solution (2.5 ml) containing 2.6 g of 5-(3-butenyl)-7-chloropyrazolo[1,5-a]pyrimidine was added dropwise while being ice-cooled. The mixture was stirred at the same temperature for another 1 hour. After completion of the reaction, water was added to the reaction mixture. The crystals precipitated were collected by filtration and washed with water and then with diethyl ether. The crude crystals obtained were recrystallized from ethyl acetate-n-hexane to provide 1.5 g of the title compound as colorless crystals. The structure and melting point of the compound obtained are shown in Table 1.

後処理

  1. temperaturecooled
  2. additionwas added dropwise
  3. temperaturecooled
  4. stirringThe mixture was stirred at the same temperature for another 1 hour
  5. additionwas added to the reaction mixture
  6. customThe crystals precipitated
  7. filtrationwere collected by filtration
  8. washwashed with water
  9. customThe crude crystals obtained
  10. customwere recrystallized from ethyl acetate-n-hexane

出典と根拠

ORDレコード
ord-4205bc1e009f4dff926864919b0a9bec
出典データセット
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05985882

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート