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Methane → 4-(Trifluoromethyl)phthalic acid

HRID 328286
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HRID 328286 반응식
[C:1]([C:3]1[CH:12]=[C:11]([C:13]([F:16])([F:15])[F:14])[CH:10]=[CH:9][C:4]=1[C:5]([O:7]C)=[O:6])#N.[OH-:17].[Na+].[OH2:19].C>CO>[F:14][C:13]([F:16])([F:15])[C:11]1[CH:12]=[C:3]([C:1]([OH:19])=[O:17])[C:4](=[CH:9][CH:10]=1)[C:5]([OH:7])=[O:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 297MethaneHCID 962WaterHCID 14798Sodium HydroxideHCID 12601887Methyl 2-cyano-4-(trifluoromethyl)benzoate

생성물 1

HCID 5990394-(Trifluoromethyl)phthalic acid

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Methyl 2-cyano-4-trifluoromethyl-benzoate (102.3 g.), sodium hydroxide pellets (108 g.), water (900 cc.) and methanol (1,900 cc.) are heated to the reflux temperature for 12 hours. The solution is decolorised by means of animal charcoal (0.6 g.). After filtration, hydrochloric acid (d = 1.19) (100 cc.) is added. The mixture is extracted with ethyl ether (2.25 liters). The organic layer is dried over anhydrous magnesium sulphate (40 g.). After filtering, and concentrating the filtrate, 4-trifluoromethyl-phthalic acid (99.1 g.) melting at 178° C is obtained.

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후처리

  1. filtrationAfter filtration, hydrochloric acid (d = 1.19) (100 cc.)
  2. additionis added
  3. extractionThe mixture is extracted with ethyl ether (2.25 liters)
  4. dry with materialThe organic layer is dried over anhydrous magnesium sulphate (40 g.)
  5. filtrationAfter filtering
  6. concentrationconcentrating the filtrate

출처 및 근거

ORD 기록
ord-78ec24dcd1a74fb9a52cc36cdc85907a
출처 데이터셋
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04016274

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