Sodium Bicarbonate → HCID 86590125, 화합물

HRID 1884917노트

반응식

HRID 1884917 반응식
[H-].[H-].[H-].[H-].[Li+].[Al+3].[Cl:7][C:8]1[CH:28]=[CH:27][C:26]([Cl:29])=[C:25]([CH3:30])[C:9]=1[C:10]([C:12]1[C:17]([CH3:18])=[CH:16][C:15]([O:19][CH3:20])=[C:14]([O:21][CH3:22])[C:13]=1[O:23][CH3:24])=[O:11].C([O-])(O)=O.[Na+]>O1CCCC1>[Cl:7][C:8]1[CH:28]=[CH:27][C:26]([Cl:29])=[C:25]([CH3:30])[C:9]=1[CH:10]([OH:11])[C:12]1[C:17]([CH3:18])=[CH:16][C:15]([O:19][CH3:20])=[C:14]([O:21][CH3:22])[C:13]=1[O:23][CH3:24]

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 11417330HCID 11417330, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 86590125HCID 86590125, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Under protective gas conditions, at about −78° C., 1 ml of a 1-molar solution of LiAlH4 in tetrahydrofuran was added dropwise to a solution of 0.37 g of 2,5-dichloro-6,6′-dimethyl-2′, 3′, 4′-trimethoxybenzophenone in 20 ml of anhydrous tetrahydrofuran, and the mixture was stirred for about 1 hour. At 20-25° C., sat. NaHCO3 solution was added to the reaction solution, the solution was extracted with ethyl acetate and the organic phase was washed with water and sat. NaCl solution and dried, and the solvent was then distilled off. The residue gave, after purification by column chromatography (mobile phase: ethyl acetate/cyclohexane 1:9), 150 mg of the title compound as a yellow viscous oil.

후처리

  1. extractionthe solution was extracted with ethyl acetate
  2. washthe organic phase was washed with water and sat. NaCl solution
  3. customdried
  4. distillationthe solvent was then distilled off
  5. customThe residue gave
  6. customafter purification by column chromatography (mobile phase: ethyl acetate/cyclohexane 1:9), 150 mg of the title compound as a yellow viscous oil

출처 및 근거

ORD 기록
ord-36847311ec9a451ea48f55015d3839f3
출처 데이터셋
uspto-grants-2004_07
특허 번호
US06767923B2

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