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

HRID 1067648
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HRID 1067648 반응식
[CH2:1]([O:3][C:4]([C:6]1[C:11]2[CH:12]=[C:13]([N+:16]([O-])=O)[CH:14]=[CH:15][C:10]=2[O:9][C:8]([CH2:21][F:22])([CH2:19][F:20])[CH:7]=1)=[O:5])[CH3:2].[Cl-].[Na+]>C(O)C>[CH2:1]([O:3][C:4]([C:6]1[C:11]2[CH:12]=[C:13]([NH2:16])[CH:14]=[CH:15][C:10]=2[O:9][C:8]([CH2:21][F:22])([CH2:19][F:20])[CH:7]=1)=[O:5])[CH3:2]
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참가 물질

4

반응물 2

HCID 5234Sodium ChlorideHCID 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 2,2-bisfluoromethyl-6-nitro-2H-1-benzopyran-4-carboxylic acid ethyl ester, 88 g of stannous chloride and 500 ml of ethyl alcohol was heated to reflux for 2 hours. The reaction mixture was combined with an aqueous 2N sodium chloride solution and extracted with ethyl acetate. The organic layer was washed with saturated saline, then dried over sodium sulfate and concentrated under reduced pressure to give 5.2 g of 6-amino-2,2-bisfluoromethyl-2H-1-benzopyran-4-carboxylic acid ethyl ester as an oil;

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 2 hours
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with saturated saline
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-76511a1ac55044028b7f56406f5e73b6
출처 데이터셋
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06248777B1

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