Aluminium lithium hydride → HCID 59334486、化合物

HRID 1639835ノート

反応式

HRID 1639835 の反応式
[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

参加物

8

反応物 2

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

生成物 1

HCID 59334486HCID 59334486、化合物収率 92%

試薬・触媒・溶媒 5

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-d824e62b529a4cb195bd1230e60a96b1
出典データセット
uspto-grants-2012_02
特許番号
US08110585B2

反応ノート

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