Phenacyl bromide → 6,6-Dimethyl-8-Keto-2-Phenyl-5,6,7,8-Tetrahydroimidazo[2,1-b]Benzothiazole

HRID 223437

反応式

HRID 223437 の反応式
[NH2:1][C:2]1[S:3][C:4]2[C:10](=[O:11])[CH2:9][C:8]([CH3:13])([CH3:12])[CH2:7][C:5]=2[N:6]=1.Br[CH2:15][C:16]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=O>C(Cl)(Cl)Cl>[CH3:12][C:8]1([CH3:13])[CH2:7][C:5]2[N:6]3[CH:15]=[C:16]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)[N:1]=[C:2]3[S:3][C:4]=2[C:10](=[O:11])[CH2:9]1

参加物

4

反応物 2

HCID 6259Phenacyl bromideHCID 5878742-Amino-5,5-dimethyl-5,6-dihydro-4H-benzothiazol-7-one

生成物 1

HCID 9143496,6-Dimethyl-8-Keto-2-Phenyl-5,6,7,8-Tetrahydroimidazo[2,1-b]Benzothiazole

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A 0.08 m. quantity each of 2-amino-5,5-dimethyl-7-keto-4,5,6,7-tetrahydrobenzothiazole and α-bromoacetophenone are mixed in 150 ml. of chloroform and heated at reflux for 4 hours. The slurry is filtered hot and the insoluble intermediate product is suspended in 600 ml. of water containing 25 g. of sodium acetate. This suspension is heated slowly to boil over 21/2 hours, then allowed to cool. The product is filtered off, washed well with water and dried yielding 12.5 g. of product melting at 175°-178° C. and having the structure: ##STR9##

後処理

  1. temperatureat reflux for 4 hours
  2. filtrationThe slurry is filtered hot
  3. temperatureThis suspension is heated slowly
  4. custom2 hours
  5. temperatureto cool
  6. filtrationThe product is filtered off
  7. washwashed well with water
  8. customdried
  9. customyielding 12.5 g

出典と根拠

ORDレコード
ord-d33b617395a44d15bdfce6aea95b21bf
出典データセット
uspto-grants-1982_10
特許番号
US04354970

関連ノート

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