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

4-Toluenesulfonyl chloride → 6-(Dimethylaminomethyl)furo[3,2-c]pyridine

HRID 1383004
ノート
印刷プレビュー

反応式

HRID 1383004 の反応式
[CH2:1]([N:3](CC)[CH2:4]C)C.C1(C)C=CC(S(Cl)(=O)=O)=CC=1.O[CH2:20][C:21]1[N:26]=[CH:25][C:24]2[CH:27]=[CH:28][O:29][C:23]=2[CH:22]=1>C(Cl)Cl>[CH3:1][N:3]([CH2:20][C:21]1[N:26]=[CH:25][C:24]2[CH:27]=[CH:28][O:29][C:23]=2[CH:22]=1)[CH3:4]
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 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 14005234Furo[3,2-c]pyridin-6-ylmethanol

生成物 1

HCID 143721506-(Dimethylaminomethyl)furo[3,2-c]pyridine収率 55.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of triethylamine (3.45 mL, 24.7 mmol) in methylene chloride (16 mL) under a nitrogen atmosphere and cooled below 5° C. was added p-toluenesulfonyl chloride (4.65 g, 24.4 mmol) in one portion. After stirring the mixture for 15 minutes, a solution of 6-hydroxymethylfuro[3,2-c]pyridine (2.68 g, 18 mmol) in methylene chloride (18 mL) was added dropwise. By tlc the reaction was complete in 6-8 hours. Dimethylamine gas was bubbled over the reaction surface until product formation was complete. The reaction solution was washed with water and the product extracted into dilute hydrochloric acid. The acidic aqueous extract was made basic with sodium hydroxide solution and the product extracted into diethyl ether. The ethereal solution was dried over anhydrous sodium sulfate, filtered through a pad of charcoal and evaporated to give an oil (1.76 g). The oil was distilled under vacuum to give 1.56 g (49% yield) of pure product, bp: 93°-94° C./1.6 mm Hg. Upon standing the product crystallized, mp: 42°-44° C.

後処理

  1. waitwas complete in 6-8 hours
  2. customDimethylamine gas was bubbled over the reaction surface until product formation
  3. washThe reaction solution was washed with water
  4. extractionthe product extracted into dilute hydrochloric acid
  5. extractionThe acidic aqueous extract
  6. extractionthe product extracted into diethyl ether
  7. dry with materialThe ethereal solution was dried over anhydrous sodium sulfate
  8. filtrationfiltered through a pad of charcoal
  9. customevaporated

出典と根拠

ORDレコード
ord-478dedd8064e4691ba3650f502a4a05c
出典データセット
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04808595

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