Hydrochloric Acid → (1S,3aS,5S,7aR)-1-[(E)-2-aminoethoxyiminomethyl]-7a-methyl-5-phenyl-2,3,4,5,6,7-hexahydro-1H-inden-3a-ol

HRID 725175노트

반응식

HRID 725175 반응식
Cl.Cl.[NH2:3][CH2:4][CH2:5][O:6][NH2:7].C([O-])(=O)C.[Na+].Cl.[CH:14]([C@@H:16]1[C@:24]2([CH3:25])[C@@:19]([OH:32])([CH2:20][C@@H:21]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)[CH2:22][CH2:23]2)[CH2:18][CH2:17]1)=O.C([O-])([O-])=O.[Na+].[Na+]>O1CCOCC1.O>[NH2:3][CH2:4][CH2:5][O:6]/[N:7]=[CH:14]/[C@@H:16]1[C@:24]2([CH3:25])[C@@:19]([OH:32])([CH2:20][C@@H:21]([C:26]3[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=3)[CH2:22][CH2:23]2)[CH2:18][CH2:17]1

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 517045Sodium AcetateHCID 11054353(1S,3aS,5S,7aR)-1-formyl-5-phenyl-7a-methylperhydroinden-3a-olHCID 143623262-(O-aminooxy)ethylamine dihydrochloride

생성물 1

HCID 10958069(1S,3aS,5S,7aR)-1-[(E)-2-aminoethoxyiminomethyl]-7a-methyl-5-phenyl-2,3,4,5,6,7-hexahydro-1H-inden-3a-ol수율 69.4%

시약·촉매·용매 2

HCID 962Water용매2회HCID 312751,4-Dioxane용매2회

실험 절차

To a solution of 6.30 g of 0.12 g of 2-aminoethoxyamine dihydrochloride, 0.28 g of sodium acetate in 2 ml of dioxane and 1 ml of water was made aid to pH 4.5 with 3N HCl. A solution of 0.20 g of (1S,3aS,5S,7aR)-1-formyl-5-phenyl -7a-methylperhydroinden-3a-ol in 1 ml of dioxane and 0.5 ml of water was added dropwise at room temperature. After 1 hr the solution was alkalinized with 10% aqueous Na2CO3 and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and evaporated to dryness. The crude product was ground with diethyl ether to give 0.17 g of the title compound (I-am) as a white solid.

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. customevaporated to dryness

출처 및 근거

ORD 기록
ord-0ed5ac84fe694c92b3957fa6fcc6899b
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05705531

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