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Hydrochloric Acid → HCID 54191570、化合物

HRID 728105
ノート
印刷プレビュー

反応式

HRID 728105 の反応式
[Cl-].Cl[CH2:3][C:4](=O)[CH2:5][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[NH2:26][C:27]1[CH:32]=[C:31]([CH3:33])[CH:30]=[CH:29][N:28]=1.[CH2:34]([O:41][C:42]1[CH:43]=[C:44]([CH:47]=[CH:48][C:49]=1[N+:50]([O-:52])=[O:51])[CH:45]=O)[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1.C(=O)([O-])[O-].[K+].[K+].Cl>C(#N)C.O>[CH2:34]([O:41][C:42]1[CH:43]=[C:44]([CH:45]=[CH:5][C:4]2[N:26]=[C:27]3[CH:32]=[C:31]([CH3:33])[CH:30]=[CH:29][N:28]3[CH:3]=2)[CH:47]=[CH:48][C:49]=1[N+:50]([O-:52])=[O:51])[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 15332-Amino-4-methylpyridineHCID 11430Potassium Carbonate2 回HCID 27736283-Chloro-2-oxopropyl triphenylphosphonium chlorideHCID 121117193-(Benzyloxy)-4-nitrobenzaldehyde

生成物 1

HCID 54191570HCID 54191570、化合物収率 45.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

実験手順

A mixture of (chloroacetonyl)triphenylphosphonium chloride (190.7 g) and 2-amino-4-methylpyridine (158.9 g) in acetonitrile (1.3 l) was stirred under reflux for 5.5 hours. To the reaction mixture were added water (400 ml) and 3-benzyloxy-4-nitrobenzaldehyde (63.0 g) under ice-cooling. The mixture was adjusted to pH 9.5 with potassium carbonate and stirred for 2.5 hours at ambient temperature under keeping the pH 9.5 to 10.0 with 20% aqueous potassium carbonate. The reaction mixture was adjusted to pH 2.0 with conc. hydrochloric acid and the precipitate was collected by filtration. To a mixture of ethyl acetate, tetrahydrofuran and water was added the above obtained precipitate and the resultant mixture was adjusted to pH 7.0 with 20% aqueous potassium carbonate. The separated organic layer was washed with brine and dried over magnesium sulfate. The solvent was removed in vacuo to give 2-[2-(3-benzyloxy-4-nitrophenyl)vinyl]-7-methylimidazo[1,2-a]pyridine (43.14 g).

後処理

  1. temperatureunder reflux for 5.5 hours
  2. temperaturecooling
  3. stirringstirred for 2.5 hours at ambient temperature
  4. filtrationthe precipitate was collected by filtration
  5. additionTo a mixture of ethyl acetate, tetrahydrofuran and water
  6. additionwas added the above obtained precipitate
  7. washThe separated organic layer was washed with brine
  8. dry with materialdried over magnesium sulfate
  9. customThe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-87938e24a82a4465a7dfa21c333e36c3
出典データセット
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05047411

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