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Acetic Acid → 2-Iodo-4-(methoxycarbonyl)-1-triphenylmethylimidazole

HRID 1108276
ノート
印刷プレビュー

反応式

HRID 1108276 の反応式
[C-]#N.[Na+].[C:4](O)(=[O:6])C.[I:8][C:9]1[N:10]([C:16]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:11]=[C:12]([CH:14]=[O:15])[N:13]=1>CO.[O-2].[O-2].[Mn+4]>[I:8][C:9]1[N:10]([C:16]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=2)[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH:11]=[C:12]([C:14]([O:6][CH3:4])=[O:15])[N:13]=1
参加物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 187846372-Iodo-4-formyl-1-triphenylmethylimidazole

生成物 1

HCID 187846292-Iodo-4-(methoxycarbonyl)-1-triphenylmethylimidazole収率 92%

試薬・触媒・溶媒 2

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

実験手順

To a mixture of activated manganese dioxide (5.66 g, 65 mmol), sodium cyanide (833 mg, 17 mmol), and glacial acetic acid (300 mg) in methanol (70 mL) was added 2-iodo-4-formyl-1-triphenylmethylimidazole (2.33 g, 5.0 mmol) in one portion. The mixture was stirred for 1 hour at room temperature and then filtered through Celite. The filtrate was concentrated and the residue was partitioned into methylene chloride and water. The organic phase was dried (magnesium sulfate) and concentrated in vacuo to give a white foamy solid. Purification by column chromatography using ethyl acetate:hexanes (1:2) afforded 2-iodo-4-(methoxycarbonyl)-1-triphenylmethylimidazole (2.26 g, 92%) as a white solid, mp 192-194° C. 1H NMR (CDCl3) δ 7.55 (s, 1H), 7.37-7.29 (m, 9H), 7.18-7.09 (m, 6H), 3.84 (s, 3H).

後処理

  1. filtrationfiltered through Celite
  2. concentrationThe filtrate was concentrated
  3. customthe residue was partitioned into methylene chloride and water
  4. dry with materialThe organic phase was dried (magnesium sulfate)
  5. concentrationconcentrated in vacuo
  6. customto give a white foamy solid
  7. customPurification by column chromatography

出典と根拠

ORDレコード
ord-cf8ea541e88e4790a29872701343f54e
出典データセット
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06066639

反応ノート

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