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

HRID 1713653

反応式

HRID 1713653 の反応式
[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

参加物

4

反応物 2

HCID 33ChloroacetaldehydeHCID 6675494-Thioureidoanisole

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-73cbf53bae11469aa911c9e263bd879e
出典データセット
uspto-grants-2010_09
特許番号
US07795288B2

関連ノート

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