Potassium Carbonate → HCID 86727412、化合物

HRID 519047ノート

反応式

HRID 519047 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 86727412HCID 86727412、化合物収率 50%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-0df583ad44e94cab8d6dceac8e5fc4f5
出典データセット
uspto-grants-2015_08
特許番号
US09115151B2

反応ノート

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