1-Bromo-2-methylpropane → HCID 23023853、化合物

HRID 851858ノート

反応式

HRID 851858 の反応式
[CH2:1](Br)[CH:2]([CH3:4])[CH3:3].[OH:6][C:7]1[CH:16]=[CH:15][C:10]([C:11]([O:13][CH3:14])=[O:12])=[CH:9][C:8]=1[N+:17]([O-:19])=[O:18].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH2:1]([O:6][C:7]1[CH:16]=[CH:15][C:10]([C:11]([O:13][CH3:14])=[O:12])=[CH:9][C:8]=1[N+:17]([O-:19])=[O:18])[CH:2]([CH3:4])[CH3:3]

参加物

5

反応物 3

HCID 65551-Bromo-2-methylpropaneHCID 11430Potassium CarbonateHCID 66835Benzoic acid, 4-hydroxy-3-nitro-, methyl ester

生成物 1

HCID 23023853HCID 23023853、化合物収率 87.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

Isobutyl bromide (10.5 mL, 95.8 mmol) was added to a suspension of methyl 4-hydroxy-3-nitrobenzoate (6.26 g, 31.8 mmol) and potassium carbonate (13.2 g, 95.5 mmol) in dry DMF (40 mL). The resulting mixture was stirred at 90° C. for 44 hours and then cooled to room temperature. Subsequently, ice-water (80 mL) was added to the cooled mixture. The precipitated crystalline product was collected by filtration, washed with water (50 mL), and dried for 30 min in air. The dried crystalline product was then washed with hexane (40 mL), and dried in air to give 7.03 g (yield 87%) of the desired compound in the form of a pale orange crystalline product.

後処理

  1. temperaturecooled to room temperature
  2. filtrationThe precipitated crystalline product was collected by filtration
  3. washwashed with water (50 mL)
  4. customdried for 30 min in air
  5. washThe dried crystalline product was then washed with hexane (40 mL)
  6. customdried in air

出典と根拠

ORDレコード
ord-3fcf96dfff4447e282df2f0c1bd68b9d
出典データセット
uspto-grants-2007_08
特許番号
US07253154B2

反応ノート

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