Acetic Acid → HCID 86683163, 화합물

HRID 920946노트

반응식

HRID 920946 반응식
[Cl:1][C:2]1[C:3]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:4]([C:8](OCC)=[O:9])[CH:5]=[N:6][CH:7]=1.[H-].C([Al+]CC(C)C)C(C)C.C(O)(=O)C.CC(=O)OCC>C1(C)C=CC=CC=1.CCCCCC>[Cl:1][C:2]1[CH:7]=[N:6][CH:5]=[C:4]([CH:8]=[O:9])[C:3]=1[C:13]([O:15][CH2:16][CH3:17])=[O:14]

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 8857Ethyl AcetateHCID 21225700DiisobutylaluminumhydrideHCID 866831643,4-Pyridinedicarboxylic acid, 5-chloro-, 3,4-diethyl ester

생성물 1

HCID 86683163HCID 86683163, 화합물수율 100.3%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8058Hexane용매

실험 절차

To a solution of diethyl 5-chloropyridine-3,4-dicarboxylate (2.43 g, 9.43 mmol) in 100 mL of toluene was added diisobutylaluminiumhydride (2.68 g, 18.86 mL, 1 molar) in hexane at −70° C. The reaction mixture was stirred for 2 h at this temperature. The reaction mixture was poured into an 5% aqueous acetic acid solution followed by the addition of EA. The phases were separated and the organic phase was washed with aq. NaHCO3 solution. The organic phase was dried and concentrated to give 2.02 g (100%) of the title compound as brown oil.

후처리

  1. customThe phases were separated
  2. washthe organic phase was washed with aq. NaHCO3 solution
  3. customThe organic phase was dried
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-9b8b3a86d3dd4f55a8c32bf62028e73a
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09273068B2

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