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Water → 1-Bromo-4-fluoro-2-methoxy-5-(methylsulfanylmethyl)benzene

HRID 575582
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HRID 575582 반응식
[CH3:1][S-:2].[Br:3][C:4]1[CH:9]=[C:8]([CH2:10]Br)[C:7]([F:12])=[CH:6][C:5]=1[O:13][CH3:14].O.C(OCC)(=O)C>CN(C=O)C>[Br:3][C:4]1[CH:9]=[C:8]([CH2:10][S:2][CH3:1])[C:7]([F:12])=[CH:6][C:5]=1[O:13][CH3:14]
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참가 물질

6

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 519392MercaptomethanideHCID 978894395-Bromo-2-fluoro-4-methoxybenzyl bromide

생성물 1

HCID 1180222021-Bromo-4-fluoro-2-methoxy-5-(methylsulfanylmethyl)benzene수율 99%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Thiomethoxide (1.19 g, 17.0 mmol) was added to a solution of 1-bromo-5-(bromomethyl)-4-fluoro-2-methoxybenzene (4.9 g, 16.4 mmol) in anhydrous DMF (25 mL) at 0° C. The mixture was stirred at room temperature for 5 h, and then poured into water (40 mL). Extractive work up with ethyl acetate gave the title compound (4.3 g, 99.0%) as colorless oil which was carried on without purification. 1H NMR (CDCl3, 400 MHz) δ 7.50 (d, J=8.0 Hz, 1H), 6.64 (d, J=11.2 Hz, 1H), 3.88 (s, 3H), 3.63 (s, 2H), 2.04 (s, 3H).

출처 및 근거

ORD 기록
ord-be59ea13747b4da19013697f5ded70d7
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09034900B2

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