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Dimethylformamide dimethyl acetal → HCID 67278716, 화합물

HRID 40710
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HRID 40710 반응식
[C:1]([C:4]1[CH:5]=[CH:6][C:7]([F:16])=[C:8]([N:10]([CH3:15])[S:11]([CH3:14])(=[O:13])=[O:12])[CH:9]=1)(=[O:3])[CH3:2].CO[CH:19](OC)[N:20]([CH3:22])[CH3:21]>CCCCCC>[CH3:19][N:20]([CH3:22])[CH:21]=[CH:2][C:1]([C:4]1[CH:5]=[CH:6][C:7]([F:16])=[C:8]([N:10]([CH3:15])[S:11]([CH3:14])(=[O:13])=[O:12])[CH:9]=1)=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 78373Dimethylformamide dimethyl acetalHCID 23160555HCID 23160555, 화합물

생성물 1

HCID 67278716HCID 67278716, 화합물수율 67.4%

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

1.66 g (6.77 mmol) of N-(5-acetyl-2-fluoro-phenyl)-N-methyl-methanesulfonamide were dissolved in 3.35 ml (3.0 g) (25.18 mmol) of N,N-dimethylformamide dimethylacetal and the resultant solution was refluxed for 2.5 hours. The mixture was cooled at room temperature. To the solid formed was added 20 ml of n-hexane and filtered to yield a solid which was crystallized from ethyl acetate. 1.37 g of N-[5-(3-dimethylamino-acryloyl)-2-fluoro-phenyl]-N-methyl-methanesulfonamide as a yellowish-white solid were obtained (yield 67.4%).

후처리

  1. customTo the solid formed
  2. filtrationfiltered
  3. customto yield a solid which
  4. customwas crystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-c572cadf2ce14664b9baff49140bcccf
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08530482B2

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