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'-Chloro-biphenyl-2-yl)-acetamidine hydrochloride salt

HRID 2169126
ノート
印刷プレビュー

反応式

HRID 2169126 の反応式
[NH4+:1].[Cl-].C[Al](C)C.[Cl:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[CH2:20][C:21]#[N:22]>C1(C)C=CC=CC=1>[ClH:7].[Cl:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[CH2:20][C:21]([NH2:1])=[NH:22]
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 16682925TrimethylaluminumHCID 86725778(2'-Chloro-biphenyl-2-yl)-acetonitrile

生成物 1

HCID 867257832-(2'-Chloro-biphenyl-2-yl)-acetamidine hydrochloride salt

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

To a stirred suspension of NH4Cl (1.4 g, 26.43 mmol) in dry toluene (40 mL) was added tri-methyl aluminium (2M in toluene, 13.2 mL, 26.43 mmol) at 5° C. The reaction mixture was then warmed to room temperature and stirred for 2 h. A solution of (2′-chloro-biphenyl-2-yl)-acetonitrile (15) (2 g, 8.8 mmol) in toluene (10 mL) was added to the reaction mixture, which was then 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 then filtered through a sintered funnel. The silica gel was washed with methanol and the combined filtrates were concentrated under reduced pressure to get 2-(2′-chloro-biphenyl-2-yl)-acetamidine hydrochloride salt as a crude product (5-02) (2 g, 80.97%) as a white solid.

後処理

  1. stirringwas then stirred 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 filtrates were concentrated under reduced pressure

出典と根拠

ORDレコード
ord-75d44b27ab1441629009e9b413a90f9b
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