Potassium Carbonate → HCID 21438986、化合物

HRID 329204

反応式

HRID 329204 の反応式
[CH2:1]([O:3][C:4]1[S:5][C:6]([C:10]#[N:11])=[C:7]([OH:9])[N:8]=1)[CH3:2].C(=O)([O-])[O-].[K+].[K+].[P:18](Cl)([O:22][CH3:23])([O:20][CH3:21])=[O:19]>CC(C)=O>[CH2:1]([O:3][C:4]1[S:5][C:6]([C:10]#[N:11])=[C:7]([O:9][P:18]([O:22][CH3:23])([O:20][CH3:21])=[O:19])[N:8]=1)[CH3:2]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 101863Phosphorochloridic acid, dimethyl esterHCID 214389692-Ethoxy-4-hydroxythiazole-5-carbonitrile

生成物 1

HCID 21438986HCID 21438986、化合物収率 57.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 17 g of 2-ethoxy-4hydroxy-5-cyano-thiazole, 14 g of potassium carbonate, 13 g of O,O-dimethyl chlorophosphate and 150 ml of acetone was stirred for 3 hours at room temperature and the mixture was concentrated to dryness. The residue was added to an aqueous sodium chloride solution which was then extracted with ethyl ether. The ether extracts were washed with an aqueous 2% sodium hydroxide solution, dried and evaporated to dryness to obtain 14.4 g of 2-ethoxy-4-dimethoxyphosphoryloxy-5-cyano-thiazole as an oil with a refractive index n D 23 = 1.5056.

後処理

  1. concentrationthe mixture was concentrated to dryness
  2. additionThe residue was added to an aqueous sodium chloride solution which
  3. extractionwas then extracted with ethyl ether
  4. washThe ether extracts were washed with an aqueous 2% sodium hydroxide solution
  5. customdried
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-d75fb1e8e60041f89ca8905dde25c868
出典データセット
uspto-grants-1977_04
特許番号
US04020076

関連ノート

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