Tetrahydrofuran → HCID 67010113, 화합물

HRID 2194536노트

반응식

HRID 2194536 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].O1CCCC1.[CH3:12][O:13][C:14]1[N:19]=[CH:18][C:17]([NH:20][C:21]2[N:30]=[CH:29][CH:28]=[CH:27][C:22]=2[C:23](OC)=[O:24])=[CH:16][CH:15]=1.[OH-].[Na+]>C(OCC)(=O)C>[CH3:12][O:13][C:14]1[N:19]=[CH:18][C:17]([NH:20][C:21]2[C:22]([CH2:23][OH:24])=[CH:27][CH:28]=[CH:29][N:30]=2)=[CH:16][CH:15]=1

참가 물질

6

반응물 4

HCID 8028Tetrahydrofuran2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 67009514Methyl 2-(6-methoxy-3-pyridinyl)aminonicotinate

생성물 1

HCID 67010113HCID 67010113, 화합물수율 101.9%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

Under a nitrogen gas stream, 2.1 g (56 mmol) of lithium aluminum hydride was added to tetrahydrofuran (100 mL) under ice cooling, and a tetrahydrofuran (60 mL) solution of 6.8 g (28 mmol) of methyl 2-(6-methoxy-3-pyridinyl)aminonicotinate was added dropwise to the above solution. The resulting mixture was stirred for 2 hours at room temperature. Ethyl acetate was added to the reaction mixture, and 23 mL of a 10% aqueous solution of sodium hydroxide was further added thereto. Insoluble materials were filtered off. The filtrate was concentrated, and the residue was dissolved in ethyl acetate, dried, filtered, and concentrated. 6.6 g of the title compound was obtained as a yellow viscous product (yield: quantitative).

후처리

  1. additionwas further added
  2. filtrationInsoluble materials were filtered off
  3. concentrationThe filtrate was concentrated
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. customdried
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-a1db1013ee7842a8a0a6bb0304a5e181
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08334236B2

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