Ethyl oxoacetate → HCID 19699373、化合物

HRID 1735889

反応式

HRID 1735889 の反応式
[F:1][C:2]1[CH:11]=[C:10]([F:12])[CH:9]=[C:8]2[C:3]=1[CH2:4][CH2:5][CH:6]([NH2:13])[CH2:7]2.[C:14]([O:18][CH2:19][CH3:20])(=[O:17])[CH:15]=O>C(O)C.[Pd]>[F:1][C:2]1[CH:11]=[C:10]([F:12])[CH:9]=[C:8]2[C:3]=1[CH2:4][CH2:5][CH:6]([NH:13][CH2:15][C:14]([O:18][CH2:19][CH3:20])=[O:17])[CH2:7]2

参加物

5

反応物 2

HCID 70211Ethyl oxoacetateHCID 196994235,7-Difluoro-1,2,3,4-tetrahydronaphthalen-2-ylamine

生成物 1

HCID 19699373HCID 19699373、化合物収率 85.1%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A mixture of 5,7-difluoro-1,2,3,4-tetrahydronaphthalen-2-ylamine (6.0 g, 32.8 mmol), prepared as in Example 8, and ethyl glyoxylate (4.6 g, 36.0 mmol) in 300 mL of ethanol was hydrogenated over 10% palladium on carbon (0.75 g) for 10 hours. The mixture was filtered and concentrated by evaporation. Purification of the residue by column chromatography on silica gel (elution: 30% ethyl acetate/hexane) gave ethyl [(5,7-difluoro-1,2,3,4-tetrahydronaphthalen-2-yl)amino]acetate (7.5 g, 27.9 mmol) as an oil.

後処理

  1. filtrationThe mixture was filtered
  2. concentrationconcentrated by evaporation
  3. customPurification of the residue by column chromatography on silica gel (elution: 30% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-49ad4b2a4d8048c5bde41066338906c9
出典データセット
uspto-grants-1996_07
特許番号
US05538988

関連ノート

読み込み中…