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Sodium Hydroxide → ethyl 6-amino-2,2-bisfluoromethyl-2H-1-benzopyran-4-carboxylate

HRID 264822
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HRID 264822 반응식
[F:1][CH2:2][C:3]1([CH2:21][F:22])[CH:8]=[C:7]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[C:6]2[CH:14]=[C:15]([N+:18]([O-])=O)[CH:16]=[CH:17][C:5]=2[O:4]1.[OH-].[Na+]>C(O)C>[NH2:18][C:15]1[CH:16]=[CH:17][C:5]2[O:4][C:3]([CH2:2][F:1])([CH2:21][F:22])[CH:8]=[C:7]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[C:6]=2[CH:14]=1
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 19037092ethyl 2,2-bisfluoromethyl-6-nitro-2H-1-benzopyran-4-carboxylate

생성물 1

HCID 19037020ethyl 6-amino-2,2-bisfluoromethyl-2H-1-benzopyran-4-carboxylate수율 13.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 42.0 g of ethyl 2,2-bisfluoromethyl-6-nitro-2H-1-benzopyran-4-carboxylate, 88 g of stannous chloride and 500 ml of ethyl alcohol was heated while refluxing for 2 hours. A 2N aqueous solution of sodium hydroxide was added to the reaction mixture, followed by extracting with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate and then concentrated under (reduced pressure to obtain 5,2 g of ethyl 6-amino-2,2-bisfluoromethyl-2H-1-benzopyran-4-carboxylate as an oily substance.

후처리

  1. temperaturewas heated
  2. temperaturewhile refluxing for 2 hours
  3. extractionby extracting with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under (reduced pressure

출처 및 근거

ORD 기록
ord-4904dceed09b407faaf0133f4df99657
출처 데이터셋
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05646310

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