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Bromine → HCID 15580980、化合物

HRID 443892
ノート
印刷プレビュー

反応式

HRID 443892 の反応式
O[CH:2]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH2:3][NH:4][C:5]([NH:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=[S:6].BrBr>ClC(Cl)(Cl)Cl>[C:14]1([CH:2]2[N:7]3[C:5]([S:6][C:9]4[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=43)=[N:4][CH2:3]2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24408BromineHCID 2873543HCID 2873543、化合物

生成物 1

HCID 15580980HCID 15580980、化合物収率 22%

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

A mixture of 50 parts of N-(2-hydroxy-2-phenylethyl)N'-phenylthiourea, 30 parts of bromine and 800 parts tetrachloromethane is stirred and refluxed for 2 hours. The reaction mixture is evaporated. From the residue, the free base is liberated in the conventional manner with ammonium hydroxide and extracted with trichloromethane. The extract is dried, filtered and evaporated. The residue is suspended in boiling 4-methyl-2-pentanone. The product is filtered off and stirred in a diluted sodium hydroxide solution. The product is extracted with 4-methyl-2-pentanone. The extract is washed with water, dried, filtered and evaporated. The residue is crystallized from acetonitrile. The product is filtered off and dried, yielding 10 parts (22%) of 2,3-dihydro-3-phenylimidazo[2,1-b]benzothiazole; mp. 131.7° C.

後処理

  1. temperaturerefluxed for 2 hours
  2. customThe reaction mixture is evaporated
  3. extractionextracted with trichloromethane
  4. customThe extract is dried
  5. filtrationfiltered
  6. customevaporated
  7. filtrationThe product is filtered off
  8. stirringstirred in a diluted sodium hydroxide solution
  9. extractionThe product is extracted with 4-methyl-2-pentanone
  10. washThe extract is washed with water
  11. customdried
  12. filtrationfiltered
  13. customevaporated
  14. customThe residue is crystallized from acetonitrile
  15. filtrationThe product is filtered off
  16. customdried

出典と根拠

ORDレコード
ord-1f081ba92a65461fa92fb52ee9915208
出典データセット
uspto-grants-1981_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04262004

反応ノート

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