4-Chloro-4'-isopropylbutyrophenone → 1-Butanone, 1-[4-(1-bromo-1-methylethyl)phenyl]-4-chloro-

HRID 1018073

반응식

HRID 1018073 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:12]=[CH:11][C:10]([CH:13]([CH3:15])[CH3:14])=[CH:9][CH:8]=1)=[O:6].[Br:16]([O-])(=O)=O.[Na+].[Br-].[Na+]>C(Cl)Cl.O.S(S([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+]>[Br:16][C:13]([C:10]1[CH:9]=[CH:8][C:7]([C:5](=[O:6])[CH2:4][CH2:3][CH2:2][Cl:1])=[CH:12][CH:11]=1)([CH3:15])[CH3:14]

참가 물질

7

반응물 3

HCID 987444-Chloro-4'-isopropylbutyrophenoneHCID 253881Sodium BromideHCID 23668195Sodium Bromate

생성물 1

HCID 100635791-Butanone, 1-[4-(1-bromo-1-methylethyl)phenyl]-4-chloro-수율 281.5%

시약·촉매·용매 3

HCID 146045Sodium dithionate촉매HCID 962Water용매HCID 6344Dichloromethane용매

반응 조건

온도
10 °C

실험 절차

Dissolve 4-chloro-1-(4-isopropyl-phenyl)-butan-1-one (74.7 g, 333 mmol) in methylene chloride (250 mL) and add sodium bromate (17.6 g, 117 mmol) in water (75 mL) in a three-necked Morton flask equipped with an overhead stirrer. Cool the solution to 10° C. and irradiate with two 150 W incandescent flood lamps. Add, by dropwise addition, a solution of sodium bromide (24 g, 233 mmol) and stir for 2 hours. Illuminate for another 30 minutes, add sodium dithionate (2.0 g), separate the organic phase, dry (MgSO4) and evaporate the solvent in vacuo to give the title compound (100 g, 99%).

후처리

  1. customequipped with an overhead stirrer
  2. customirradiate with two 150 W incandescent flood lamps
  3. additionAdd, by dropwise addition
  4. customIlluminate for another 30 minutes
  5. customseparate the organic phase
  6. dry with materialdry (MgSO4)
  7. customevaporate the solvent in vacuo

출처 및 근거

ORD 기록
ord-7b2b8f69c1a0413696162a20122ef69b
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06479663B2

연결된 노트

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