Bromine → 6-Bromo-8-fluoro-4,4-dimethyl-dihydro-benzo[d][1,3]oxazin-2-one

HRID 1634971

반응식

HRID 1634971 반응식
[F:1][C:2]1[CH:3]=[CH:4][CH2:5][CH:6]2[C:11]([CH3:13])([CH3:12])[O:10][C:9](=[O:14])[NH:8][C:7]=12.[Br:15]Br>C(O)(=O)C>[Br:15][C:4]1[CH2:5][CH:6]2[C:11]([CH3:12])([CH3:13])[O:10][C:9](=[O:14])[NH:8][C:7]2=[C:2]([F:1])[CH:3]=1

참가 물질

4

반응물 2

HCID 24408BromineHCID 68822414HCID 68822414, 화합물

생성물 1

HCID 688225046-Bromo-8-fluoro-4,4-dimethyl-dihydro-benzo[d][1,3]oxazin-2-one수율 84%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

To a solution of 8-fluoro-4,4-dimethyl-dihydro-benzo[d][1,3]oxazin-2-one (0.15 g, 0.77 mmol) in acetic acid (5 mL) was added dropwise a solution of bromine (0.37 g, 2.31 mmol) in acetic acid (5 mL) under nitrogen at rt. After stirring for 10 minutes, the mixture was concentrated and the residue obtained was purified by a silica gel column (hexane:ethyl acetate/4:1) to afford 6-bromo-8-fluoro-4,4-dimethyl-dihydro-benzo[d][1,3]oxazin-2-one as an off-white solid (0.176 g, 84%) which was used in next step without further purification.

후처리

  1. concentrationthe mixture was concentrated
  2. customthe residue obtained
  3. customwas purified by a silica gel column (hexane:ethyl acetate/4:1)

출처 및 근거

ORD 기록
ord-81462d3aa2a042c48a1db939420d9e36
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06509334B1

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