1-Bromo-2-methylpropane → HCID 23023853, 화합물

HRID 851858노트

반응식

HRID 851858 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 23023853HCID 23023853, 화합물수율 87.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
90 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3fcf96dfff4447e282df2f0c1bd68b9d
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07253154B2

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