Water → HCID 16667230, 화합물

HRID 1927598

반응식

HRID 1927598 반응식
Br[C:2]1[CH:18]=[CH:17][C:5]([C:6]([NH:8][CH2:9][C:10]2[C:11]([CH3:16])=[N:12][O:13][C:14]=2[CH3:15])=[O:7])=[CH:4][C:3]=1[F:19].Br[C:21]1[CH:29]=[CH:28][C:24]([C:25](O)=O)=[CH:23][C:22]=1F.[C:31](Cl)([C:33](Cl)=O)=O.CC1[C:42]([CH2:43][NH2:44])=C(C)ON=1.[OH2:46]>ClCCCl.CN(C=O)C>[CH2:6]([N:8]([CH2:31][CH3:33])[C:9]([CH:25]([C:24]1[CH:28]=[CH:29][CH:21]=[CH:22][CH:23]=1)[N:44]1[CH2:43][CH2:42][N:12]([C:2]2[CH:18]=[CH:17][C:5]([C:6]([NH:8][CH2:9][C:10]3[C:11]([CH3:16])=[N:12][O:13][C:14]=3[CH3:15])=[O:7])=[CH:4][C:3]=2[F:19])[CH2:11][CH2:10]1)=[O:46])[CH3:5]

참가 물질

8

반응물 5

HCID 962WaterHCID 65578Oxalyl chlorideHCID 27733414-Bromo-3-fluorobenzoic acidHCID 11018874(Dimethyl-1,2-oxazol-4-yl)methanamineHCID 69304057HCID 69304057, 화합물

생성물 1

HCID 16667230HCID 16667230, 화합물수율 69%

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매HCID 6228Dimethylformamide용매

실험 절차

4-Bromo-N-(3,5-dimethyl-isoxazol-4-ylmethyl)-3-fluoro-benzamide. To a mixture of 4-bromo-3-fluoro-benzoic acid (3.0 mmol) and DMF (0.10 mL) in DCE (10 mL) was added (COCl)2 (4.0 mL) dropwise. After 30 min, the mixture was concentrated and dried under vacuum. The residue was dissolved in DCE (20 mL), treated with C-(3,5-dimethyl-isoxazol-4-yl)-methylamine (3.0 mmol) and TEA (8.0 mmol), and stirred at rt for 16 h. The mixture was treated with H2O (10 mL). The resulting precipitate was collected by filtration to give the title compound (650 mg, 69%).

후처리

  1. concentrationthe mixture was concentrated
  2. customdried under vacuum
  3. dissolutionThe residue was dissolved in DCE (20 mL)
  4. filtrationThe resulting precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-10aa7b6ad7d0451c86b4cf2781b44f7c
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08183239B2

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