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Sodium Hydroxide → HCID 12496842, 화합물

HRID 1155308
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HRID 1155308 반응식
[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
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참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 35455FeprazoneHCID 61456Phosphoric acid, disodium salt, dodecahydrate

생성물 1

HCID 12496842HCID 12496842, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c71ce10a7600448ab11264140972e776
출처 데이터셋
uspto-grants-1981_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04301177

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