(S)-1-(2-Fluorophenyl)ethylamine → HCID 178462012, 화합물

HRID 339870

반응식

HRID 339870 반응식
[Br:1][C:2]1[CH:3]=[C:4]([C:8]2([CH3:20])[C:13]([CH3:15])([CH3:14])[O:12][C:11](OC)=[N:10][S:9]2(=[O:19])=[O:18])[CH:5]=[CH:6][CH:7]=1.[F:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[C@@H:28]([NH2:30])[CH3:29]>C(Cl)Cl>[Br:1][C:2]1[CH:3]=[C:4]([C:8]2([CH3:20])[C:13]([CH3:15])([CH3:14])[O:12][C:11]([NH:30][C@H:28]([C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=3[F:21])[CH3:29])=[N:10][S:9]2(=[O:19])=[O:18])[CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 7023579(S)-1-(2-Fluorophenyl)ethylamineHCID 683591715-(3-Bromophenyl)-2-methoxy-5,6,6-trimethyl-5,6-dihydro-1,4,3-oxathiazine 4,4-dioxide

생성물 1

HCID 178462012HCID 178462012, 화합물수율 62.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 209 mg of 5-(3-bromophenyl)-2-methoxy-5,6,6-trimethyl-5,6-dihydro-1,4,3-oxathiazine 4,4-dioxide and 92 mg of (S)-1-(2-fluorophenyl)ethylamine in 5 ml of methylene chloride was stirred at room temperature for 1 hour and the conversion was checked by LCMS. Since no conversion had taken place yet, the solvent was concentrated by rotary evaporation and the residue was stirred at room temperature for 19 hours. The crude product was purified by means of normal phase chromatography using a Flashmaster with an n-heptane/ethyl acetate gradient. The product-containing fractions were combined and concentrated by rotary evaporation. This gave the product (170 mg) with a molecular weight of 469.4 g/mol (C20H22BrFN2O3S); MS (ESI): m/e=469 (M+H+).

후처리

  1. concentrationthe solvent was concentrated by rotary evaporation
  2. customThe crude product was purified by means of normal phase chromatography
  3. concentrationconcentrated by rotary evaporation

출처 및 근거

ORD 기록
ord-d90dd1d3fdd44c2e9bf407e0efe1df8a
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08895547B2

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