Chloroacetonitrile → HCID 13961736, 화합물

HRID 256339노트

반응식

HRID 256339 반응식
[OH:1][C:2]1[C:11]([O:12][CH3:13])=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].[C:14](=O)([O-])[O-].[K+].[K+].Cl[CH2:21][C:22]#[N:23]>CN(C)C=O>[C:22]([CH2:21][CH2:14][O:1][C:2]1[C:11]([O:12][CH3:13])=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5])#[N:23]

참가 물질

5

반응물 3

HCID 7856ChloroacetonitrileHCID 11430Potassium CarbonateHCID 80651Methyl 3-methoxysalicylate

생성물 1

HCID 13961736HCID 13961736, 화합물수율 77%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 57.1 g (0.31 mole) of 2-hydroxy-3-methoxybenzoic acid, methyl ester, 95.5 g (0.69 mole) of anhydrous potassium carbonate, and 23.9 ml (28.5 g; 0.38 mole) of chloroacetonitrile in 260 ml of N,N-dimethylformamide is heated on the steam bath for three hours. The mixture is cooled, added to 1700 g of ice/water, stirred for 1 hour, and the precipitated crude product is filtered and washed with water. Recrystallization from aqueous methanol yields 52.5 g 77% yield) of the 2-cyanoethoxy-3-methoxybenzoic acid, methyl ester, mp 77°-78° C. (See U.S. Pat. No. 4,420,476 for mp of 74°-75° C.)

후처리

  1. temperatureis heated on the steam bath for three hours
  2. temperatureThe mixture is cooled
  3. customthe precipitated crude product
  4. filtrationis filtered
  5. washwashed with water
  6. customRecrystallization from aqueous methanol

출처 및 근거

ORD 기록
ord-c202b639c696456fb101ec787bee625b
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04703053

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