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

Ammonium Chloride → 2-(2,3-Dichlorophenyl)-acetamidine hydrochloride

HRID 2169214
ノート
印刷プレビュー

反応式

HRID 2169214 の反応式
[NH4+:1].[Cl-].C[Al](C)C.[Cl:7][C:8]1[C:13]([Cl:14])=[CH:12][CH:11]=[CH:10][C:9]=1[CH2:15][C:16]#[N:17]>C1(C)C=CC=CC=1>[ClH:7].[Cl:7][C:8]1[C:13]([Cl:14])=[CH:12][CH:11]=[CH:10][C:9]=1[CH2:15][C:16]([NH2:1])=[NH:17]
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 25517Ammonium ChlorideHCID 229020Benzeneacetonitrile, 2,3-dichloro-HCID 16682925Trimethylaluminum

生成物 1

HCID 867258632-(2,3-Dichlorophenyl)-acetamidine hydrochloride収率 156.2%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

To a stirred suspension of NH4Cl (4.29 g, 80.21 mmol) in dry toluene (120 mL) was added trimethyl aluminium (2M in toluene, 41 mL, 80.21 mmol) at 5° C. The mixture was then warmed to room temperature and stirred for 2 h. A solution of (2,3-dichlorophenyl)-acetonitrile (128) (5 g, 26.73 mmol) in toluene (25 mL) was added to the mixture and stirred for 14 h at 80° C. After completion of the reaction, it was quenched with a suspension of silica gel in chloroform and the reaction mixture was stirred for half an hour at room temperature and filtered through a sintered funnel. The silica gel was washed with methanol and the combined filtrate was concentrated under reduced pressure to get 2-(2,3-dichlorophenyl)-acetamidine hydrochloride salt (129) (5 g, 78%) as an off-white solid.

後処理

  1. stirringstirred for 14 h at 80° C
  2. customAfter completion of the reaction, it
  3. customwas quenched with a suspension of silica gel in chloroform
  4. stirringthe reaction mixture was stirred for half an hour at room temperature
  5. filtrationfiltered through a sintered funnel
  6. washThe silica gel was washed with methanol
  7. concentrationthe combined filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-386af2cc10cb4841a0f700214c6a1749
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09045486B2

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