3-Nitrobenzaldehyde → 2-Hydroxyethyl 3,4,5,8-tetrahydro-6-methyl-8-(3-nitrophenyl)-1,1-dioxo-2H-thiopyrano [3,2-b]pyridine-7-carboxylate

HRID 231348ノート

反応式

HRID 231348 の反応式
[S:1]1(=[O:9])(=[O:8])[CH2:6][CH2:5][CH2:4][C:3](=O)[CH2:2]1.[N+:10]([C:13]1[CH:14]=[C:15]([CH:18]=[CH:19][CH:20]=1)[CH:16]=O)([O-:12])=[O:11].[OH:21][CH2:22][CH2:23][O:24][C:25](=[O:30])/[CH:26]=[C:27](\[NH2:29])/[CH3:28].C([O-])(=O)C.[NH4+]>C(O)C>[CH3:28][C:27]1[NH:29][C:3]2[CH2:4][CH2:5][CH2:6][S:1](=[O:9])(=[O:8])[C:2]=2[CH:16]([C:15]2[CH:18]=[CH:19][CH:20]=[C:13]([N+:10]([O-:12])=[O:11])[CH:14]=2)[C:26]=1[C:25]([O:24][CH2:23][CH2:22][OH:21])=[O:30]

参加物

6

反応物 4

HCID 74493-NitrobenzaldehydeHCID 517165Ammonium AcetateHCID 11815935Dihydro-2H-thiopyran-3(4H)-one-1,1-dioxideHCID 19980851HCID 19980851、化合物

生成物 1

HCID 140112132-Hydroxyethyl 3,4,5,8-tetrahydro-6-methyl-8-(3-nitrophenyl)-1,1-dioxo-2H-thiopyrano [3,2-b]pyridine-7-carboxylate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of tetrahydrothiopyran-3-one-1,1-dioxide (2.80 g, 0.0189 moles), 3-nitrobenzaldehyde (2.85 g, 0.0189 moles), 2-hydroxyethyl-3-aminocrotonate (3.28 g, 0.0226 moles), ammonium acetate (0.291 g, 0.0038 moles) and ethanol (35 mL) was refluxed for 16 hours. After cooling to room temperature the resulting solid was isolated by filtration, washed with ethanol and diethyl ether. The product was dried under vacuum for 16 hours at room temperature affording the product; mp 233°-235° C.

後処理

  1. temperaturewas refluxed for 16 hours
  2. customwas isolated by filtration
  3. washwashed with ethanol and diethyl ether
  4. customThe product was dried under vacuum for 16 hours at room temperature
  5. customaffording the product

出典と根拠

ORDレコード
ord-fca93793333646b4ac4f9ad83b353c20
出典データセット
uspto-grants-1989_07
特許番号
US04845225

反応ノート

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