ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

1-Bromopropane → HCID 13339929、化合物

HRID 2418682
ノート
印刷プレビュー

反応式

HRID 2418682 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[CH:11]=[N:10][CH:9]([CH3:12])[N:5]2[C:6](=[O:8])[N:7]=1.[H-].[Na+].Br[CH2:16][CH2:17][CH3:18]>O1CCOCC1>[Cl:1][C:2]1[N:7]([CH2:16][CH2:17][CH3:18])[C:6](=[O:8])[N:5]2[C:9]([CH3:12])=[N:10][CH:11]=[C:4]2[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 78401-BromopropaneHCID 24758Sodium hydrideHCID 70454969HCID 70454969、化合物

生成物 1

HCID 13339929HCID 13339929、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a mixture of 2.0 g (10.9 mmole) of 7-chloro-3-methylimidazo[1,5-c]pyrimidin-5-one (from Example 4, Part B) in 50 ml of dioxane was added 0.52 g (13 mmole) of 60% sodium hydride in oil. After ten minutes of stirring, 1.6 g (13 mmole) of 3-bromopropane was added and the mixture was stirred for 16 hours at 50° C. The solution was poured into 100 ml of an ice water mixture. The resulting solution was extracted four times with 75 ml portions of chloroform. The extracts were washed twice with water, dried, and evaporated. The residue was dissolved in 80 ml of chloroform, washed with six 100 ml portions of water, dried and evaporated. The residue was recrystallized with treatment with decolorizing charcoal from cyclohexane to provide 7-chloro-3-methyl-6-n-propylimidazo[1,5-c]pyrimidin-5-one, m.p. 125°-126° C. Analysis: Calculated for C10H12ClNO: %C, 53.2 ; %H, 5.4; %N, 18.6; Found: %C, 53.5; %H, 5.3; %N, 18.6.

後処理

  1. stirringthe mixture was stirred for 16 hours at 50° C
  2. extractionThe resulting solution was extracted four times with 75 ml portions of chloroform
  3. washThe extracts were washed twice with water
  4. customdried
  5. customevaporated
  6. dissolutionThe residue was dissolved in 80 ml of chloroform
  7. washwashed with six 100 ml portions of water
  8. customdried
  9. customevaporated
  10. customThe residue was recrystallized with treatment with decolorizing charcoal from cyclohexane

出典と根拠

ORDレコード
ord-14af5294041d49db8632775f0a95e610
出典データセット
uspto-grants-1984_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04473570

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート