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

Isobutylene oxide → 1-[5-(6-Chloro-2-methylpyridin-3-yl)-1H-1,2,3-triazol-1-yl]-2-methylpropan-2-ol

HRID 385974
ノート
印刷プレビュー

反応式

HRID 385974 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]([C:9]2[N:10]=[N:11][NH:12][CH:13]=2)=[CH:4][CH:3]=1.[O:14]1[C:16]([CH3:18])([CH3:17])[CH2:15]1.CC([O-])(C)C.[K+].[Cl-].[NH4+]>CN(C=O)C>[Cl:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]([C:9]2[N:10]([CH2:15][C:16]([CH3:18])([OH:14])[CH3:17])[N:11]=[N:12][CH:13]=2)=[CH:4][CH:3]=1
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 11208Isobutylene oxideHCID 25517Ammonium ChlorideHCID 23665647Potassium tert-butoxideHCID 1784328616-Chloro-2-methyl-3-(1H-1,2,3-triazol-4-yl)pyridine

生成物 1

HCID 595262551-[5-(6-Chloro-2-methylpyridin-3-yl)-1H-1,2,3-triazol-1-yl]-2-methylpropan-2-ol

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

反応条件

温度
60 °C

実験手順

6-Chloro-2-methyl-3-(1H-1,2,3-triazol-4-yl)pyridine (131 mg, 0.68 mmol) and 1,2-epoxy-2-methylpropane (65 μl, 0.71 mmol) were taken-up in DMF (2.7 ml). Potassium 2-methylpropan-2-olate (114 mg, 1.01 mmol) was added, and the mixture was heated to 60° C. for seven hours. Saturated aqueous ammonium chloride was added and the resulting mixture was extracted three times with ethyl acetate. The combined organic layers were dried over anhydrous magnesium sulfate, filtered, concentrated, purified by reverse-phase HPLC (10-100% acetonitrile/water with 0.05% trifluoroacetic acid modifier). The appropriate fractions were neutralized with aqueous sodium bicarbonate and extracted twice with ethyl acetate. The organic layers were combined, dried over anhydrous magnesium sulfate, filtered, and concentrated to afford the title compound.

後処理

  1. extractionthe resulting mixture was extracted three times with ethyl acetate
  2. dry with materialThe combined organic layers were dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. custompurified by reverse-phase HPLC (10-100% acetonitrile/water with 0.05% trifluoroacetic acid modifier)
  6. extractionextracted twice with ethyl acetate
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-8e16de72a4f94da390416b37e42a2ce7
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367706B2

反応ノート

読み込み中…

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