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

Aluminium lithium hydride → 2-(4-Chloro-2-methylphenyl)ethanamine

HRID 1048027
ノート
印刷プレビュー

反応式

HRID 1048027 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]=[CH:9][N+:10]([O-])=O)=[C:4]([CH3:13])[CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][NH2:10])=[C:4]([CH3:13])[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

4

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 670259694-Chloro-2-methyl-1-(2-nitrovinyl)benzene

生成物 1

HCID 202519552-(4-Chloro-2-methylphenyl)ethanamine収率 75%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 4-chloro-2-methyl-1-(2-nitrovinyl)benzene (1.83 g, 9.26 mmol) in tetrahydrofuran (40 mL) was cooled to 0° C. in an ice bath, and a 1M solution of lithium aluminum hydride in tetrahydrofuran (37 mL, 37 mmol) was added, dropwise over 10 minutes. The resulting mixture was stirred in the ice bath for 2 hours 30 minutes, then quenched in the following manner: water (1.5 mL) was added dropwise, and after stirring for 5 minutes, 1M sodium hydroxide (1.5 mL) was added. After stirring for a further 15 minutes, water (5 mL) was added, and the resulting mixture was stirred at ambient temperature for 15 minutes, then filtered through a medium porosity sintered glass funnel. The collected precipitate was washed with ethyl acetate (60 mL). The combined filtrate and wash was dried over sodium sulfate and concentrated to afford 2-(4-chloro-2-methylphenyl)ethanamine as a brown oil (1.17 g, 75% yield).

後処理

  1. customquenched in the following manner
  2. additionwater (1.5 mL) was added dropwise
  3. addition1M sodium hydroxide (1.5 mL) was added
  4. stirringAfter stirring for a further 15 minutes
  5. additionwater (5 mL) was added
  6. stirringthe resulting mixture was stirred at ambient temperature for 15 minutes
  7. filtrationfiltered through a medium porosity sintered glass funnel
  8. washThe collected precipitate was washed with ethyl acetate (60 mL)
  9. washThe combined filtrate and wash
  10. dry with materialwas dried over sodium sulfate
  11. concentrationconcentrated

出典と根拠

ORDレコード
ord-cbfe2d09d0b343b697b31f08d1d394bc
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08569522B2

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