2-Methylbenzoic acid → Mepronil

HRID 1287699

반응식

HRID 1287699 반응식
[CH3:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=O.[CH:11]([O:14][C:15]1[CH:16]=[C:17]([CH:19]=[CH:20][CH:21]=1)[NH2:18])([CH3:13])[CH3:12].C(N(CC)CC)C.P(Cl)(Cl)(Cl)=O>C1(C)C(C)=CC=CC=1>[CH:11]([O:14][C:15]1[CH:16]=[C:17]([CH:19]=[CH:20][CH:21]=1)[NH:18][C:4](=[O:6])[C:3]1[CH:7]=[CH:8][CH:9]=[CH:10][C:2]=1[CH3:1])([CH3:13])[CH3:12]

참가 물질

6

반응물 4

HCID 83732-Methylbenzoic acidHCID 8471TriethylamineHCID 24813Phosphorus oxychlorideHCID 5732203-Isopropoxyaniline

생성물 1

HCID 41632Mepronil수율 77.9%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

A 13.6 g (0.1 mol) portion of o-methylbenzoic acid, 15.1 g (0.1 mol) of m-isopropoxyaniline and 10.1 g (0.1 mol) of triethylamine were dissolved in 100 ml of xylene. A 5.1 g (0.033 mol) amount of phosphorus oxychloride was added dropwise to the prepared solution with stirring at 90° - 100° C. Stirring of the resulting solution was continued at 90° - 100° C for 3 hours. The reaction mixture was cooled and washed with water, and the product was dried over anhydrous sodium sulfate. The xylene was removed to obtain 20.9 g (77.9%) of white prismatic crystals having a melting point of 92°-94° C.

후처리

  1. stirringStirring of the resulting solution
  2. temperatureThe reaction mixture was cooled
  3. washwashed with water
  4. dry with materialthe product was dried over anhydrous sodium sulfate
  5. customThe xylene was removed

출처 및 근거

ORD 기록
ord-047315b6dd9645c3a248bc4d168187fd
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03985804

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