Diethyl methylmalonate → HCID 58280423、化合物

HRID 1506877ノート

反応式

HRID 1506877 の反応式
[F:1][C:2]1[CH:3]=[C:4]([N+:10]([O-:12])=[O:11])[CH:5]=[C:6]([F:9])[C:7]=1F.[CH3:13][CH:14]([C:20]([O:22][CH2:23][CH3:24])=[O:21])[C:15]([O:17][CH2:18][CH3:19])=[O:16].[OH-].[Na+]>CN(C=O)C>[F:9][C:6]1[CH:5]=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=[C:2]([F:1])[C:7]=1[C:14]([CH3:13])([C:15]([O:17][CH2:18][CH3:19])=[O:16])[C:20]([O:22][CH2:23][CH3:24])=[O:21]

参加物

5

反応物 3

HCID 11857Diethyl methylmalonateHCID 14798Sodium HydroxideHCID 27827931,2,3-Trifluoro-5-nitrobenzene

生成物 1

HCID 58280423HCID 58280423、化合物収率 76.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of commercially available 3,4,5-trifluoro-nitrobenzene (25b) (5.0 mL, 42.8 mmol), diethyl methylmalonate (6.1 mL, 35.7 mmol), and sodium hydroxide (1.54 g, 38.5 mmol) in DMF (55 mL) was allowed to react in the same manner as in (a) in Production Example 1. The crude product was subjected to silica gel column chromatography and elution with an n-hexane/ethyl acetate (10:1) solution to give 9.1 g (63%) of compound (26b) of interest as clear brown oil.

後処理

  1. washThe crude product was subjected to silica gel column chromatography and elution with an n-hexane/ethyl acetate (10:1) solution

出典と根拠

ORDレコード
ord-14129075846a4110b3e616f7e63c679b
出典データセット
uspto-grants-2015_12
特許番号
US09221786B2

反応ノート

読み込み中…