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

HRID 652057

반응식

HRID 652057 반응식
[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]

참가 물질

7

반응물 5

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-59335595239343ebbaf7e4fe817cfef8
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04670450

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