Hydrochloric Acid → 4-Ethyl-5-pyridin-4-yl-2(3H)thiazolone

HRID 652057

反応式

HRID 652057 の反応式
[N:1]1[CH:6]=[CH:5][C:4]([CH:7](Br)[C:8](=O)[CH2:9][CH3:10])=[CH:3][CH:2]=1.C([NH:16][C:17](N)=[S:18])(=O)C.[O-:20]C#N.[K+].Cl.C(=O)(O)[O-].[Na+]>C(O)C>[CH2:9]([C:8]1[NH:16][C:17](=[O:20])[S:18][C:7]=1[C:4]1[CH:5]=[CH:6][N:1]=[CH:2][CH:3]=1)[CH3:10]

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 2723593AcetylthioureaHCID 11378442Potassium cyanateHCID 201992181-(4-Pyridyl)-1-bromo-2-butanone

生成物 1

HCID 201450164-Ethyl-5-pyridin-4-yl-2(3H)thiazolone

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

1-(4-Pyridyl)-1-bromo-2-butanone (28.8 g, 0.1 mol) and 1-acetyl-2-thiourea (13.0 g, 0.11 mol) are combined in 200 ml absolute ethanol and refluxed 24 hours. The solvent is evaporated and the residue is purified by chromatography. The thiol is mixed with (8.1 g, 0.1 mol) potassium cyanate and 0.2 mol 10% aqueous hydrochloric acid. The mixture is heated to 80° C. for 15 minutes, then cooled. The acid is adjusted to ph=6.5 with solid sodium bicarbonate which causes the product to precipitate.

後処理

  1. temperaturerefluxed 24 hours
  2. customThe solvent is evaporated
  3. customthe residue is purified by chromatography
  4. temperaturecooled
  5. customto precipitate

出典と根拠

ORDレコード
ord-59335595239343ebbaf7e4fe817cfef8
出典データセット
uspto-grants-1987_06
特許番号
US04670450

関連ノート

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