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

Acetic Acid → HCID 57786311、化合物

HRID 1399211
ノート
印刷プレビュー

反応式

HRID 1399211 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH2:23])=[C:6]2[C:10]=1[N:9]=[C:8]1[N:11]([C:15]3[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:16]=3[Cl:22])[CH2:12][CH2:13][CH2:14][N:7]21.C(O[C:27]1(O[Si](C)(C)C)[CH2:29][CH2:28]1)C.[C:35]([BH3-])#N.[Na+].[C:39](O)(=O)[CH3:40]>CO.C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:23]([CH:27]2[CH2:28][CH2:29]2)[CH:40]2[CH2:39][CH2:35]2)=[C:6]2[C:10]=1[N:9]=[C:8]1[N:11]([C:15]3[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:16]=3[Cl:22])[CH2:12][CH2:13][CH2:14][N:7]21
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 176Acetic AcidHCID 2734686(1-Ethoxycyclopropoxy)trimethylsilaneHCID 5003444Sodium cyanoborohydrideHCID 577863289-Chloro-1-(2,4-dichlorophenyl)-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazol-6-amine

生成物 1

HCID 57786311HCID 57786311、化合物収率 19%

試薬・触媒・溶媒 2

HCID 887
Methanol
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 9-chloro-1-(2,4-dichlorophenyl)-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazol-6-amine (367 mg, 1.00 mmol), (1-ethoxycyclopropoxy)trimethylsilane (1.01 mL, 5.00 mmol), sodium cyanoborohydride (314 mg, 5.00 mmol), and acetic acid (572 μL, 10.0 mmol) in methanol (3.0 mL) was stirred at reflux for 40 h. The reaction mixture was diluted with ethyl acetate, quenched with aqueous sodium hydrogen carbonate, and filtrated. The organic layer was washed with brine, dried over sodium sulfate, filtered, and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel eluting with a 20% ethyl acetate/hexane mixture to give the title compound as a colorless solid (83.5 mg, 0.186 mmol, 19%). Analytically pure material was obtained by recrystallization from ethyl acetate/hexane.

後処理

  1. temperatureat reflux for 40 h
  2. customquenched with aqueous sodium hydrogen carbonate
  3. filtrationfiltrated
  4. washThe organic layer was washed with brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by flash column chromatography on silica gel eluting with a 20% ethyl acetate/hexane mixture

出典と根拠

ORDレコード
ord-8346dc4976b6453ea567739f593eb275
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08901141B2

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