Potassium Carbonate → HCID 86727412, 화합물

HRID 519047노트

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HRID 519047 반응식
[N+:1]([C:4]1[CH:14]=[CH:13][C:7]2[S:8][CH2:9][C:10](=[O:12])[NH:11][C:6]=2[CH:5]=1)([O-:3])=[O:2].Br[CH:16]([CH3:22])[C:17]([O:19][CH2:20][CH3:21])=[O:18].C([O-])([O-])=O.[K+].[K+]>CC(C)=O>[N+:1]([C:4]1[CH:14]=[CH:13][C:7]2[S:8][CH2:9][C:10](=[O:12])[N:11]([CH:16]([CH3:22])[C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:6]=2[CH:5]=1)([O-:3])=[O:2]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 79040Ethyl 2-bromopropionateHCID 41823566-Nitro-2H-benzo[b][1,4]thiazin-3(4H)-one

생성물 1

HCID 86727412HCID 86727412, 화합물수율 50%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 6-nitro-2H-benzo[b][1,4]thiazin-3(4H)-one (0.512 g, 2.436 mmol), ethyl 2-bromopropanoate (0.573 g, 3.17 mmol) and K2CO3 (1.01 g, 7.31 mmol) in acetone (40 mL) was heated at reflux for 16 h. After cooling to ambient temperature, the mixture was filtered and the filtrate was evaporated in vacuo. The residue was purified by column chromatography on silica gel (eluting with 9% EtOAc in petroleum ether) to give ethyl 2-(6-nitro-3-oxo-2H-benzo[b][1,4]thiazin-4(3H)-yl)propanoate (0.376 g, 50%). TLC (eluting with 20% EtOAc/PE) Rf=0.6.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 16 h
  3. filtrationthe mixture was filtered
  4. customthe filtrate was evaporated in vacuo
  5. customThe residue was purified by column chromatography on silica gel (eluting with 9% EtOAc in petroleum ether)

출처 및 근거

ORD 기록
ord-0df583ad44e94cab8d6dceac8e5fc4f5
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115151B2

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