Diethyl methylmalonate → HCID 58280423, 화합물

HRID 1506877노트

반응식

HRID 1506877 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 58280423HCID 58280423, 화합물수율 76.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-14129075846a4110b3e616f7e63c679b
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09221786B2

반응 노트

불러오는 중…