Water → Methyl alpha,alpha-Dimethyl-9-nitro-9,10-dihydroanthracene-10-acetate

HRID 542995

반응식

HRID 542995 반응식
[N+:1]([C:4]1[C:5]2[C:10]([CH:11]=[C:12]3[C:17]=1[CH:16]=[CH:15][CH:14]=[CH:13]3)=[CH:9][CH:8]=[CH:7][CH:6]=2)([O-:3])=[O:2].CSS(C)(=O)=O.CN([S+](N(C)C)N(C)C)C.[CH3:34][Si-](F)(F)(C)C.[OH2:40].[CH2:41]1[CH2:45][O:44][CH2:43][CH2:42]1>C(#N)C>[CH3:34][C:42]([CH3:41])([CH:11]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]([N+:1]([O-:3])=[O:2])[C:17]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]1=2)[C:43]([O:44][CH3:45])=[O:40]

참가 물질

7

반응물 5

HCID 962WaterHCID 8028TetrahydrofuranHCID 117679-NitroanthraceneHCID 18064S-Methyl methanethiosulfonateHCID 9795567Tris(dimethylamino)sulfonium difluorotrimethylsilicate2회

생성물 1

HCID 13507921Methyl alpha,alpha-Dimethyl-9-nitro-9,10-dihydroanthracene-10-acetate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of 1.115 g (5 mmol) of 9-nitroanthracene and 1.01 mL (5 mmol) of MMTS in 20 mL of anhydrous THF was treated with 1.375 g (5 mmol) of TASF dissolved in 3 mL of acetonitrile at -78° C. After addition of TASF had been completed, the reaction mixture was brought to -10° C. and stirred for 1 hr. Ten mL of water was then added, the mixture was warmed to room temperature, and the product was extracted into ether. The organic layer was washed with saturated sodium chloride solution, dried and concentrated. The melting point was 159° to 163° C. (dec). The product material was analyzed by ultraviolet absorption, infrared spectroscopy, nuclear magnetic resonance spectroscopy, and mass spectrometry.

후처리

  1. customwas brought to -10° C.
  2. extractionthe product was extracted into ether
  3. washThe organic layer was washed with saturated sodium chloride solution
  4. customdried
  5. concentrationconcentrated
  6. customThe product material was analyzed by ultraviolet absorption

출처 및 근거

ORD 기록
ord-f95d76ad56e54d6bb7abcc7ba8eaf04e
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04659862

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