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Hydrochloric Acid → 2-Isopropyl-4-trifluoromethyl-benzoic acid

HRID 1950924
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HRID 1950924 반응식
[I-].[CH:2]([C:5]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[CH:7][C:6]=1[C:15]1[O:16]CC(C)(C)[N+]=1C)([CH3:4])[CH3:3].[OH-:23].[Na+].Cl>CO>[CH:2]([C:5]1[CH:10]=[C:9]([C:11]([F:12])([F:13])[F:14])[CH:8]=[CH:7][C:6]=1[C:15]([OH:16])=[O:23])([CH3:3])[CH3:4]
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 666828202-(2-Isopropyl-4-trifluoromethyl-phenyl)-3,4,4-trimethyl-4,5-dihydro-oxazol-3-ium iodide

생성물 1

HCID 594385402-Isopropyl-4-trifluoromethyl-benzoic acid수율 90.3%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
75 °C

실험 절차

To a solution of 2-(2-isopropyl-4-trifluoromethyl-phenyl)-3,4,4-trimethyl-4,5-dihydro-oxazol-3-ium iodide (step 2) (1.26 g, 2.949 mmol) in 12 ml methanol were added 5N NaOH solution (11.8 ml, 58.98 mmol). The mixture was stirred in a 75° C. oil bath for 3 hours. The solution was cooled in an ice bath and acidified to pH 1 with a 5N HCl solution. The methanol was removed in vacuo. The suspension was stirred in an ice bath. The solid was filtered, washed with water and dried in vacuo to provide 618 mg (90%) of the title compound as a white solid. MS (m/e): 231.1 (M−H).

후처리

  1. temperatureThe solution was cooled in an ice bath
  2. customThe methanol was removed in vacuo
  3. stirringThe suspension was stirred in an ice bath
  4. filtrationThe solid was filtered
  5. washwashed with water
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-fe697d493da0493d86d2d06f6bd27418
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08404673B2

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