Water → Trifop-methyl

HRID 1414113

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HRID 1414113 반응식
S(OC)(O[CH3:5])(=O)=O.[F:8][C:9]([F:30])([F:29])[C:10]1[CH:28]=[CH:27][C:13]([O:14][C:15]2[CH:26]=[CH:25][C:18]([O:19][CH:20]([CH3:24])[C:21]([O-:23])=[O:22])=[CH:17][CH:16]=2)=[CH:12][CH:11]=1.[Na+].O.OP(O)(O)=O>C1(C)C(C)=CC=CC=1>[CH3:5][O:22][C:21](=[O:23])[CH:20]([O:19][C:18]1[CH:25]=[CH:26][C:15]([O:14][C:13]2[CH:12]=[CH:11][C:10]([C:9]([F:29])([F:30])[F:8])=[CH:28][CH:27]=2)=[CH:16][CH:17]=1)[CH3:24]

참가 물질

6

반응물 4

HCID 962WaterHCID 1004Phosphoric AcidHCID 6497Dimethyl SulfateHCID 23675546HCID 23675546, 화합물

생성물 1

HCID 94586Trifop-methyl

시약·촉매·용매 1

HCID 7237O-Xylene용매

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온도
85 °C

실험 절차

63 g of dimethyl sulfate are added within 5 minutes and at 130° C. to 348 g of anhydrous sodium-2-[4'-(4"-trifluoromethyl-phenoxy)-phenoxy]-propionate, suspended in 1,000 ml of xylene. After the addition, stirring of the mixture is continued for 1 hour, the mixture is cooled at 85° C., at said temperature 200 ml of water and 0.5 ml of H3PO4 are added and, for the separation of the inorganic salts, the mixture is stirred for 10 minutes. After separation of the water phase, the xylene is distilled off. 340 g of methyl-2-[4'-(4"-trifluoromethyl-phenoxy)-phenoxy]-propionate are obtained melting at 142° C. under 0.05 torr. According to gas chromatogram the content of pure final product is 99.4%, the residual content of unreacted acid is 0.6%, which corresponds to a yield of 99.4%.

후처리

  1. additionAfter the addition
  2. additionare added and, for the separation of the inorganic salts
  3. stirringthe mixture is stirred for 10 minutes
  4. customAfter separation of the water phase
  5. distillationthe xylene is distilled off

출처 및 근거

ORD 기록
ord-4c4ffb351c7643d1bc21a5c46786903b
출처 데이터셋
uspto-grants-1981_02
특허 번호
US04252980

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