Tetrahydrofuran → HCID 67010113、化合物

HRID 2194536ノート

反応式

HRID 2194536 の反応式
[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

参加物

6

反応物 4

HCID 8028Tetrahydrofuran2 回HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 67009514Methyl 2-(6-methoxy-3-pyridinyl)aminonicotinate

生成物 1

HCID 67010113HCID 67010113、化合物収率 101.9%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a1db1013ee7842a8a0a6bb0304a5e181
出典データセット
uspto-grants-2012_12
特許番号
US08334236B2

反応ノート

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