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HCID 90229603, 화합물 → HCID 90229275, 화합물

HRID 1505764
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인쇄 미리보기

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HRID 1505764 반응식
[F:1][C:2]([F:27])([F:26])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]([NH:11][C:12]1[CH:13]=[C:14]([C:21]([O:23]CC)=[O:22])[C:15]2[O:19][CH2:18][CH2:17][C:16]=2[CH:20]=1)=[O:10]>CCO.[OH-].[Na+]>[F:26][C:2]([F:1])([F:27])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]([NH:11][C:12]1[CH:13]=[C:14]([C:21]([OH:23])=[O:22])[C:15]2[O:19][CH2:18][CH2:17][C:16]=2[CH:20]=1)=[O:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 90229603HCID 90229603, 화합물

생성물 1

HCID 90229275HCID 90229275, 화합물수율 95.7%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 14798Sodium Hydroxide용매

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온도
80 °C

실험 절차

To a suspension of ethyl 5-({[2-(trifluoromethyl)phenyl]carbonyl}amino)-2,3-dihydro-1-benzofuran-7-carboxylate (220 mg) obtained in Step 2 in EtOH (5 mL), 1N aqueous sodium hydroxide solution (1 mL) was added and the mixture was stirred at 80° C. for 4 hours. The reaction mixture was cooled to room temperature, and EtOH was removed under reduced pressure. To the residue was added water, and the solution was acidified to pH 3 with 1N hydrochloric acid under ice-cooling and extracted with ethyl acetate. The organic layer was washed sequentially with water and brine, dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure to obtain the titled compound (195 mg) as slightly yellow powder.

후처리

  1. additionwas added
  2. temperatureThe reaction mixture was cooled to room temperature
  3. customEtOH was removed under reduced pressure
  4. additionTo the residue was added water
  5. temperaturecooling
  6. extractionextracted with ethyl acetate
  7. washThe organic layer was washed sequentially with water and brine
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-4b65986685884212a4348b4cbe52e09e
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216968B2

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