Triethylamine → 2,4-dichloro-6-fluoro-7-[N-(2,2-dimethylpropanoyl)hydrazino]benzothiazole

HRID 21733노트

반응식

HRID 21733 반응식
C(N(CC)CC)C.[Cl:8][C:9]1[S:10][C:11]2[C:17]([NH:18][NH2:19])=[C:16]([F:20])[CH:15]=[C:14]([Cl:21])[C:12]=2[N:13]=1.[C:22](Cl)(=[O:27])[C:23]([CH3:26])([CH3:25])[CH3:24].C(OCC)(=O)C>C1(C)C=CC=CC=1>[Cl:8][C:9]1[S:10][C:11]2[C:17]([N:18]([C:22](=[O:27])[C:23]([CH3:26])([CH3:25])[CH3:24])[NH2:19])=[C:16]([F:20])[CH:15]=[C:14]([Cl:21])[C:12]=2[N:13]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 62493Pivaloyl chlorideHCID 199334672,4-Dichloro-6-fluoro-7-hydrazinobenzothiazole

생성물 1

HCID 199334582,4-dichloro-6-fluoro-7-[N-(2,2-dimethylpropanoyl)hydrazino]benzothiazole

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

2.6 ml Triethylamine was added to a solution of 4.8 g 2,4-dichloro-6-fluoro-7-hydrazinobenzothiazole in 38 ml toluene. 2.4 ml Pivaloyl chloride was added dropwise and the mixture stirred for 2 hours at room temperature. It was then treated with ethyl acetate and washed with aqueous sodium hydrogen carbonate and water, dried over magnesium sulfate and concentrated. The residue was purified by column chromatography. Yield: 1.36 g=21% of theory

후처리

  1. washwashed with aqueous sodium hydrogen carbonate and water
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-3507dce14f7b4406b6930ba5b945d4f0
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05424443

반응 노트

불러오는 중…