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Sodium Hydroxide → HCID 12496842、化合物

HRID 1155308
ノート
印刷プレビュー

反応式

HRID 1155308 の反応式
[CH3:1][C:2]([CH3:24])=[CH:3][CH2:4][CH:5]1[C:9](=[O:10])[N:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:7]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:6]1=[O:23].[OH-].[Na+].O.O.O.O.O.O.O.O.O.O.O.O.P([O-])([O-])(O)=[O:40].[Na+].[Na+]>O>[C:11]1([N:8]([C:9](=[O:10])[CH:5]([CH2:4][CH:3]=[C:2]([CH3:24])[CH3:1])[C:6]([OH:23])=[O:40])[NH:7][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1
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 14798Sodium HydroxideHCID 35455FeprazoneHCID 61456Phosphoric acid, disodium salt, dodecahydrate

生成物 1

HCID 12496842HCID 12496842、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

103.8 gm (0.324 mol) of 4-(3-methyl-2-butenyl)-1,2-diphenyl-3,5-dioxopyrazolidine were dissolved in a solution of 12.96 gm (0.324 mol) of sodium hydroxide pellets and 57.3 gm (0.16 mol) of disodium hydrogen phosphate dodecahydrate in 400 ml of water. The reaction mixture was heated for 30 hours in an atmosphere of nitrogen, then cooled, diluted with 600 ml of water, and filtered. The filtered solution was neutralized (pH 7 to 7.5) with 2 N hydrochloric acid and extracted several times with chloroform. The combined chloroform extracts were evaporated, leaving crude 2-(3-methyl-2-butenyl)propanedioic acid mono(1,2-diphenylhydrazide) which was dissolved in 500 ml of 10% aqueous ammonium hydroxide. To this solution a solution of 17.9 gm (0.162 mol) of calcium chloride in 50 ml of water was added while stirring.

後処理

  1. temperatureThe reaction mixture was heated for 30 hours in an atmosphere of nitrogen
  2. temperaturecooled
  3. filtrationfiltered
  4. extractionextracted several times with chloroform
  5. customThe combined chloroform extracts were evaporated

出典と根拠

ORDレコード
ord-c71ce10a7600448ab11264140972e776
出典データセット
uspto-grants-1981_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04301177

反応ノート

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