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

HRID 1018073

反応式

HRID 1018073 の反応式
[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]

参加物

7

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 146045Sodium dithionate触媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
10 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-7b2b8f69c1a0413696162a20122ef69b
出典データセット
uspto-grants-2002_11
特許番号
US06479663B2

関連ノート

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