Iodoethane → HCID 86699746, 화합물

HRID 515178노트

반응식

HRID 515178 반응식
[Br:1][C:2]1[CH:10]=[C:9]([CH3:11])[C:5]([C:6]([OH:8])=[O:7])=[C:4]([O:12][CH3:13])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:20](I)[CH3:21]>CN(C=O)C.O>[CH2:20]([O:7][C:6](=[O:8])[C:5]1[C:9]([CH3:11])=[CH:10][C:2]([Br:1])=[CH:3][C:4]=1[O:12][CH3:13])[CH3:21]

참가 물질

6

반응물 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 454803864-Bromo-2-methoxy-6-methylbenzoic acid

생성물 1

HCID 86699746HCID 86699746, 화합물수율 89%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To a stirred solution of 4-bromo-2-methoxy-6-methyl-benzoic acid (synthesized according to the methods described in sections a) to d) of example 10) (10.7 g, 43.7 mmol) in DMF (90 ml) are added potassium carbonate (12.1 g, 87.3 mmol) and ethyl iodide (17.5 ml, 218 mmol) and the resulting mixture is stirred at room temperature for 2 h. After completion of reaction the reaction mixture is diluted with water (200 ml) and extracted with ethyl acetate (3×50 ml). The combined organic layers are washed with water (2×30 ml), brine (2×30 ml), dried over sodium sulfate and concentrated in vacuo yielding 4-bromo-2-methoxy-6-methyl-benzoic acid ethyl ester (10.5 g, 39 mmol, 89%).

후처리

  1. customAfter completion of reaction the reaction mixture
  2. extractionextracted with ethyl acetate (3×50 ml)
  3. washThe combined organic layers are washed with water (2×30 ml), brine (2×30 ml)
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-3674c076dace4675a5d2b55f58989bb4
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09108936B2

반응 노트

불러오는 중…