Water → Benzoic acid, 3-methoxy-2-nitro-, methyl ester

HRID 576325

반응식

HRID 576325 반응식
[CH3:1][O:2][C:3]1[C:4]([N+:12]([O-:14])=[O:13])=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([OH:8])=[O:7].[C:15]([O-])([O-])=O.[K+].[K+].CI.O>CN(C=O)C>[CH3:1][O:2][C:3]1[C:4]([N+:12]([O-:14])=[O:13])=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([O:8][CH3:15])=[O:7]

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 786323-Methoxy-2-nitrobenzoic acid

생성물 1

HCID 79195Benzoic acid, 3-methoxy-2-nitro-, methyl ester

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a mixture of 3-methoxy-2-nitrobenzoic acid (25.0 g, 126 mmol) and K2CO3 (35.0 g, 253 mmol) in DMF (126 mL) was added MeI (15.8 mL, 253 mmol) at room temperature. The mixture was stirred at room temperature for 2 hours. To the mixture was poured the water (200 mL) and then stirred at 5° C. for 30 min. The precipitated solid was collected by filtration, washed with water and hexane. The solid was dried under reduced pressure to afford the compound 52 in a crude form (26.2 g, 98%) as a white solid.

후처리

  1. stirringstirred at 5° C. for 30 min
  2. filtrationThe precipitated solid was collected by filtration
  3. washwashed with water and hexane
  4. customThe solid was dried under reduced pressure

출처 및 근거

ORD 기록
ord-fb38c9e1c3204998875316fa067af5e4
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09034921B2

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