Chloroacetaldehyde → (4-Methoxy-phenyl)thiazol-2-yl-amine

HRID 1713653

반응식

HRID 1713653 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]([NH2:12])=[S:11])=[CH:5][CH:4]=1.Cl[CH2:14][CH:15]=O>CCO>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([NH:9][C:10]2[S:11][CH:14]=[CH:15][N:12]=2)=[CH:7][CH:8]=1

참가 물질

4

반응물 2

HCID 33ChloroacetaldehydeHCID 6675494-Thioureidoanisole

생성물 1

HCID 956680(4-Methoxy-phenyl)thiazol-2-yl-amine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of (4-methoxy-phenyl)-thiourea (3.0 g, 16.5 mmol) and a 45% aqueous solution of chloroacetaldehyde (12 mL, 82.4 mmol, 5.0 equiv) in EtOH (23 mL) is heated to reflux for 1 h. The resulting dark orange solution is allowed to cool to RT and concentrated in vacuo. NaHCO3 is then added to the oily residue until CO2 evolution subsides and a beige precipitate forms. The product is collected by vacuum filtration, washed thoroughly with water (600 mL), and dried in vacuo. Title compound: ES-MS: 207.0 [M+H]+; single peak at tR=5.32 min (System 1); Rf=0.17 (CH2Cl2/MeOH, 95/5).

후처리

  1. temperatureto reflux for 1 h
  2. concentrationconcentrated in vacuo
  3. additionNaHCO3 is then added to the oily residue until CO2 evolution subsides
  4. filtrationThe product is collected by vacuum filtration
  5. washwashed thoroughly with water (600 mL)
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-73cbf53bae11469aa911c9e263bd879e
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07795288B2

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