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Hydrochloric Acid → HCID 54107311, 화합물

HRID 2296692
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HRID 2296692 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:18]([NH:21]C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=[CH:19][CH:20]=1)[C:5]([OH:17])([C:10]#[C:11][C:12]1[O:13][CH:14]=[CH:15][CH:16]=1)[C:6]([F:9])([F:8])[F:7].Cl.C(=O)(O)[O-]>CO>[NH2:21][C:18]1[C:4]([C:5]([OH:17])([C:10]#[C:11][C:12]2[O:13][CH:14]=[CH:15][CH:16]=2)[C:6]([F:7])([F:8])[F:9])=[CH:3][C:2]([Cl:1])=[CH:20][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 769Bicarbonate IonHCID 15486989HCID 15486989, 화합물

생성물 1

HCID 54107311HCID 54107311, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a stirred solution of 2.0 g of 3-Chloro-6-(triphenylmethy)amino-α-(2-furanyl)ethynyl-α-(trifluoromethyl)benzyl alcohol (Example 9, Part B) in 20 mL of methanol was added 0.125 mL of 12 N aqueous hydrochloric acid, and the resulting solution was stirred at ambient temperature for 30 min. The reaction mixture was poured onto aqueous bicarbonate and extracted with ether. The ether layer was washed with brine, dried and evaporated. The residue was dissolved in methanol after cooling in ice for 1 h, the precipitated methyl trityl ether was filtered off. After evaporation of the filtrate, the residue was chromatographed over silica gel (elution with hexanes/ethyl acetate 3:1) affording after crystalization from hexane/ethyl acetate 280 mg of the title compound.

후처리

  1. extractionextracted with ether
  2. washThe ether layer was washed with brine
  3. customdried
  4. customevaporated
  5. dissolutionThe residue was dissolved in methanol
  6. temperatureafter cooling in ice for 1 h
  7. filtrationthe precipitated methyl trityl ether was filtered off
  8. customAfter evaporation of the filtrate
  9. customthe residue was chromatographed over silica gel (elution with hexanes/ethyl acetate 3:1)
  10. customaffording
  11. customafter crystalization from hexane/ethyl acetate 280 mg of the title compound

출처 및 근거

ORD 기록
ord-3bdb65be9d7f4899b991132a70049fa0
출처 데이터셋
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06489320B1

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