Aluminium lithium hydride → HCID 59334486, 화합물

HRID 1639835노트

반응식

HRID 1639835 반응식
[CH3:1][C:2]1[S:3][C:4]2[C:10]([C:11](OC)=[O:12])=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1.C(OCC)(=O)C.O.[OH-].[Na+].Cl>[CH3:1][C:2]1[S:3][C:4]2[C:10]([CH2:11][OH:12])=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1

참가 물질

8

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 450771752-Methyl-7-benzothiazolecarboxylic acid methyl ester

생성물 1

HCID 59334486HCID 59334486, 화합물수율 92%

시약·촉매·용매 5

HCID 313Hydrochloric Acid용매HCID 962Water용매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매HCID 14798Sodium Hydroxide용매

실험 절차

Under nitrogen atmosphere, to a solution of methyl 2-methyl-1,3-benzothiazole-7-carboxylate (6.00 g, 29.0 mmol) in tetrahydrofuran (150 mL) was added lithium aluminum hydride (1.18 g, 34.7 mmol) at 0° C., and the mixture was stirred at room temperature for 1 hr. The reaction mixture was diluted with ethyl acetate and water, 1 M aqueous sodium hydroxide solution (10 mL) and 2 M hydrochloric acid (10 mL) were added, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane=1/1) to give the title compound (4.78 g, yield 92%).

후처리

  1. additionwere added
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe extract was washed with saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane=1/1)

출처 및 근거

ORD 기록
ord-d824e62b529a4cb195bd1230e60a96b1
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08110585B2

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