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

1,3-Propanediamine → N-(3-aminoprop-1-yl)-3,4-dichlorobenzylamine

HRID 430087
ノート
印刷プレビュー

反応式

HRID 430087 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][NH2:5].[Cl:6][C:7]1[CH:8]=[C:9]([CH:12]=[CH:13][C:14]=1[Cl:15])[CH2:10]Cl>C1COCC1>[NH2:1][CH2:2][CH2:3][CH2:4][NH:5][CH2:10][C:9]1[CH:12]=[CH:13][C:14]([Cl:15])=[C:7]([Cl:6])[CH:8]=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 4281,3-PropanediamineHCID 76093,4-Dichlorobenzyl chloride

生成物 1

HCID 18353717N-(3-aminoprop-1-yl)-3,4-dichlorobenzylamine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To 1,3-diaminopropane (42 ml) in dry THF (200 ml) at 60° C. was added dropwise a solution of 3,4-dichlorobenzylchloride (13.9 ml, 100 mmol) in 90 ml dry THF over 3 h. The mixture was kept at 60° C. for an additional 15 min and then kept at 25° C. for 3 days. The precipitate was removed by filtration and the mother liquor concentrated in vacuo. The residue was partitioned between water and t-butyl methyl ether (TBME). To the organic layer was added aq. HCl (2 M) and the mixture was filtered. The layers were separated and NaOH was added to the aqueous layer with stirring. The resulting mixture was extracted with TBME and the organic extract was dried (Na2CO3), filtered, and the solvent evaporated to give the title compound as a slightly cloudy oil, (18.2 g, 78%). δH (CDCl3) 1.20 (br, s, ca. 3H), 1.58-1.71 (m, 2H), 2.67 (t, J=6.9, 2H), 2.78 (t, J=6.8, 2H), 3.74 (s, 2H), 7.15 (dd, J=8.2, 2.0, 1H), 7.37 (d, J=8.2, 1H), 7.43 (d, J=1.9, 1H); MS (ES+) 233 (MH+, 13%), 159 (100).

後処理

  1. waitkept at 25° C. for 3 days
  2. customThe precipitate was removed by filtration
  3. concentrationthe mother liquor concentrated in vacuo
  4. customThe residue was partitioned between water and t-butyl methyl ether (TBME)
  5. additionTo the organic layer was added aq. HCl (2 M)
  6. filtrationthe mixture was filtered
  7. customThe layers were separated
  8. additionNaOH was added to the aqueous layer
  9. extractionThe resulting mixture was extracted with TBME
  10. extractionthe organic extract
  11. dry with materialwas dried (Na2CO3)
  12. filtrationfiltered
  13. customthe solvent evaporated

出典と根拠

ORDレコード
ord-3409bdc02ad74574a3c89aab6894c1df
出典データセット
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06320051B1

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