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 15698056、化合物

HRID 465798
ノート
印刷プレビュー

反応式

HRID 465798 の反応式
[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]1[CH:15]=[CH:14][C:13]([CH2:16][N:17]2[C:21]([CH:22]=[O:23])=[C:20]([Cl:24])[N:19]=[C:18]2[CH2:25][CH2:26][CH2:27][CH3:28])=[CH:12][CH:11]=1)([OH:3])=[O:2].[C-]#N.[Na+].[C:32](O)(=[O:34])C>CO.[O-2].[O-2].[Mn+4]>[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]1[CH:11]=[CH:12][C:13]([CH2:16][N:17]2[C:21]([C:22]([O:34][CH3:32])=[O:23])=[C:20]([Cl:24])[N:19]=[C:18]2[CH2:25][CH2:26][CH2:27][CH3:28])=[CH:14][CH:15]=1)([OH:3])=[O:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 176Acetic AcidHCID 8929Sodium CyanideHCID 11625408HCID 11625408、化合物

生成物 1

HCID 15698056HCID 15698056、化合物

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 887Methanol溶媒

反応条件

温度
25 °C

実験手順

To a mixture of 1.45 g of 1-[(2'-carboxybiphenyl-4-yl)methyl]-2-butyl-4-chloroimidazole-5-carboxaldehyde and 0.91 g of sodium cyanide in 20 mL of methanol at 25° C. was added 0.32 mL of acetic acid followed by 7.25 g of manganese dioxide. The resulting mixture was stirred at 25° C. for 40 hours. The reaction mixture was filtered through Celite®, and the filtrate diluted with water. The aqueous solution was adjusted to pH 3 using hydrochloric acid and extracted with methylene chloride. The combined organic phases were washed with brine, dried over anhydrous sodium sulfate, filtered, and concentrated. The crude product was recrystallized from diethyl ether to afford 0.90 g of methyl 1-[(2'-carboxybiphenyl-4-yl)methyl]-2-butyl-4-chloroimidazole-5-carboxylate (m.p. 154°-155° C.). NMR (200 MHz, DMSO-d6); δ12.75 (br s, 1H), 7.73 (d, 1H) 7.58 (t, 1H), 7.46 (t, 1H), 7.34 (m, 3H), 7.07 (d, 2H), 5.63 (s, 2H), 3.78 (s, 3H), 2.67 (t, 2H), 1.56 (quint., 2H), 1.29 (sext., 2H), 0.83 (t, 3H).

後処理

  1. filtrationThe reaction mixture was filtered through Celite®
  2. additionthe filtrate diluted with water
  3. extractionextracted with methylene chloride
  4. washThe combined organic phases were washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe crude product was recrystallized from diethyl ether

出典と根拠

ORDレコード
ord-3e1ff35e865546648aa4cdc4329044b5
出典データセット
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05153197

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート