Hydrogen Bromide → 2-[4,5-Bis-(p-methoxyphenyl)-thiazol-2-ylthio]-acetaldehyde

HRID 544662ノート

反応式

HRID 544662 の反応式
C([O:3][C:4](=O)[CH:5]([S:8][C:9]1[S:10][C:11]([C:22]2[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[CH:24][CH:23]=2)=[C:12]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)[N:13]=1)C=O)C.Br>C(O)(=O)C>[CH3:21][O:20][C:17]1[CH:18]=[CH:19][C:14]([C:12]2[N:13]=[C:9]([S:8][CH2:5][CH:4]=[O:3])[S:10][C:11]=2[C:22]2[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[CH:24][CH:23]=2)=[CH:15][CH:16]=1

参加物

4

反応物 2

HCID 260Hydrogen BromideHCID 543019562-[4,5-Bis-(p-methoxyphenyl)-thiazol-2-ylthio]-2-formylacetic acid ethyl ester

生成物 1

HCID 132096722-[4,5-Bis-(p-methoxyphenyl)-thiazol-2-ylthio]-acetaldehyde

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

4.0 g of 2-[4,5-bis-(p-methoxyphenyl)-thiazol-2-ylthio]-2-formylacetic acid ethyl ester are dissolved in 50 ml of acetic acid, 10 ml of 43% strength hydrobromic acid are added and the mixture is heated at 80° for 4 hours. The mixture is concentrated to dryness by evaporation under reduced pressure, and the residue is dissolved in 200 ml of ethyl acetate, washed twice with 50 ml of saturated sodium bicarbonate solution each time and with water, dried over magnesium sulphate and concentrated to dryness by evaporation. The crude product is recrystallised from hexane/diethyl ether (55 ml+10 ml). 2-[4,5-bis-(p-methoxyphenyl)-thiazol-2-ylthio]-acetaldehyde having a melting point of 75°-76° is obtained.

後処理

  1. temperaturethe mixture is heated at 80° for 4 hours
  2. concentrationThe mixture is concentrated to dryness by evaporation under reduced pressure
  3. dissolutionthe residue is dissolved in 200 ml of ethyl acetate
  4. washwashed twice with 50 ml of saturated sodium bicarbonate solution each time
  5. dry with materialwith water, dried over magnesium sulphate
  6. concentrationconcentrated to dryness by evaporation
  7. customThe crude product is recrystallised from hexane/diethyl ether (55 ml+10 ml)

出典と根拠

ORDレコード
ord-7cae3f533ddd46688009f0690d0c1218
出典データセット
uspto-grants-1984_05
特許番号
US04451471

反応ノート

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