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

Pyridine → HCID 86634178、化合物

HRID 1928799
ノート
印刷プレビュー

反応式

HRID 1928799 の反応式
[CH:1]1([N:4]2[CH:9]3[CH2:10][CH2:11][CH:5]2[CH2:6][C:7](=O)[CH2:8]3)[CH2:3][CH2:2]1.N1C=CC=CC=1.Cl.[NH2:20][OH:21]>C(O)C.C([O-])([O-])=O.[Na+].[Na+]>[CH:1]1([N:4]2[CH:9]3[CH2:10][CH2:11][CH:5]2[CH2:6][C:7](=[N:20][OH:21])[CH2:8]3)[CH2:3][CH2:2]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 3

HCID 1049PyridineHCID 443297Hydroxyamine hydrochlorideHCID 204824738-Cyclopropyl-8-Azabicyclo(3.2.1)octan-3-one

生成物 1

HCID 86634178HCID 86634178、化合物収率 84%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 10340Sodium Carbonate溶媒

反応条件

温度
23 °C

実験手順

A mixture of 8-cyclopropyl-8-aza-bicyclo[3.2.1]octan-3-one (CAS no: 60206-33-9) (17.86 g, 108.08 mmol) in ethanol (500 mL) with pyridine (13.05 mL, 162.1 mmol) and hydroxylamine hydrochloride (9.764 g, 140.51 mmol) was refluxed overnight. Cooled to 23° C., filtered off, washed with ethanol and ether and dried in vacuum to give a white solid, which was suspended in 200 mL sat. Na2CO3 solution and extracted 3 times with dichloromethane, the combined organic layers were dried over Na2SO4, filtered off and evaporated totally, dried in high vacuum to give the title compound as white crystals (16.3 g, 84%); MS: m/e=181.2 (M+H+).

後処理

  1. temperaturewas refluxed overnight
  2. filtrationfiltered off
  3. washwashed with ethanol and ether
  4. customdried in vacuum
  5. customto give a white solid, which
  6. extractionextracted 3 times with dichloromethane
  7. dry with materialthe combined organic layers were dried over Na2SO4
  8. filtrationfiltered off
  9. customevaporated totally
  10. customdried in high vacuum

出典と根拠

ORDレコード
ord-370e03321b09404989c4483bb8ad8e4e
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08183380B2

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