Sodium Acetate → 1,1,1-trifluoro-2,3-butandione 3-(7-fluoro-3-oxo-4-propargyl-2H-1,4-benzoxazin-6-ylhydrazone)

HRID 2288633노트

반응식

HRID 2288633 반응식
C([O-])(=O)C.[Na+].Br[C:7](Br)([CH3:14])[C:8](=[O:13])[C:9]([F:12])([F:11])[F:10].[F:16][C:17]1[C:30]([NH:31][NH2:32])=[CH:29][C:20]2[N:21]([CH2:26][C:27]#[CH:28])[C:22](=[O:25])[CH2:23][O:24][C:19]=2[CH:18]=1>O>[F:16][C:17]1[C:30]([NH:31][N:32]=[C:7]([CH3:14])[C:8](=[O:13])[C:9]([F:12])([F:11])[F:10])=[CH:29][C:20]2[N:21]([CH2:26][C:27]#[CH:28])[C:22](=[O:25])[CH2:23][O:24][C:19]=2[CH:18]=1

참가 물질

5

반응물 3

HCID 517045Sodium AcetateHCID 118329383,3-Dibromo-1,1,1-trifluorobutan-2-oneHCID 145179487-fluoro-6-hydrazino-4-propargyl-2H-1,4-benzoxazin-3-one

생성물 1

HCID 725849421,1,1-trifluoro-2,3-butandione 3-(7-fluoro-3-oxo-4-propargyl-2H-1,4-benzoxazin-6-ylhydrazone)

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a mixed solution of 8.0 g (97.2 mmol) of sodium acetate and about 50 ml of water was added under ice cooling 6.9 g (24.3 mmol) of 3,3-dibromo-1,1,1-trifluorobutanone, and the reaction was allowed to proceed at 80° C. for 30 minutes. Then, the reaction mixture was cooled to 0° C., to which 4.4 g (18.7 mmol) of 7-fluoro-6-hydrazino-4-propargyl-2H-1,4-benzoxazin-3-one was added, and the reaction mixture was stirred at room temperature for 2 hours. The precipitated crystals were collected by filtration, washed twice with 10 ml of water, and dried, which afforded 6.1 g (17.0 mmol) of 1,1,1-trifluoro-2,3-butandione 3-(7-fluoro-3-oxo-4-propargyl-2H-1,4-benzoxazin-6-ylhydrazone).

후처리

  1. additionwas added
  2. filtrationThe precipitated crystals were collected by filtration
  3. washwashed twice with 10 ml of water
  4. customdried

출처 및 근거

ORD 기록
ord-2c80592c29f2432aa05789a7d938a7f5
출처 데이터셋
uspto-grants-2000_07
특허 번호
US06090753

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