Azane;hydrate → (3R*,4S*)-4-amino-6-methoxy-2,2-dimethyl-7-nitro-3,4-dihydro-2H-1-benzopyran-3-ol

HRID 505642노트

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HRID 505642 반응식
[O:1]1[C@H:7]2[C@@H:2]1[C:3]([CH3:18])([CH3:17])[O:4][C:5]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[C:9]([O:15][CH3:16])=[CH:8][C:6]=12.O.[NH3:20]>C(O)C>[NH2:20][C@H:7]1[C:6]2[CH:8]=[C:9]([O:15][CH3:16])[C:10]([N+:12]([O-:14])=[O:13])=[CH:11][C:5]=2[O:4][C:3]([CH3:18])([CH3:17])[C@@H:2]1[OH:1]

참가 물질

4

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HCID 12896473Azane;hydrateHCID 25196994(3R*,4R*)-3,4-epoxy-6-methoxy-2,2-dimethyl-7-nitro-3,4-dihydro-2H-1-benzopyran

생성물 1

HCID 59031749(3R*,4S*)-4-amino-6-methoxy-2,2-dimethyl-7-nitro-3,4-dihydro-2H-1-benzopyran-3-ol수율 84%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
100 °C

실험 절차

To a solution of (3R*,4R*)-3,4-epoxy-6-methoxy-2,2-dimethyl-7-nitro-3,4-dihydro-2H-1-benzopyran (2.64 g, 10.5 mmol) in ethanol (26 mL), an ammonia water (26 mL) was added, and the resulting mixture was stirred in a sealed tube at 100° C. for 2 hours. Upon the completion of the reaction, the solvent was distilled off. An aqueous solution of saturated sodium carbonate was added to the residue, and the resulting mixture was extracted with ethyl acetate. The organic phase was washed with saturated sodium chloride solution, dried over anhydrous magnesium sulfate and thereby the aimed product was obtained as red amorphous substance (yield: 84%).

후처리

  1. customUpon the completion of the reaction
  2. distillationthe solvent was distilled off
  3. additionAn aqueous solution of saturated sodium carbonate was added to the residue
  4. extractionthe resulting mixture was extracted with ethyl acetate
  5. washThe organic phase was washed with saturated sodium chloride solution
  6. dry with materialdried over anhydrous magnesium sulfate

출처 및 근거

ORD 기록
ord-0bb61f71ffe74a0184c35a136c2d5c84
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07781483B2

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