4-Chloro-alpha,alpha,alpha-trifluoro-3-nitrotoluene → 1-Propanol, 3-[[2-nitro-4-(trifluoromethyl)phenyl]amino]-

HRID 46841

反応式

HRID 46841 の反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].[NH2:15][CH2:16][CH2:17][CH2:18][OH:19]>C(O)CCC>[N+:12]([C:3]1[CH:4]=[C:5]([C:8]([F:11])([F:10])[F:9])[CH:6]=[CH:7][C:2]=1[NH:15][CH2:16][CH2:17][CH2:18][OH:19])([O-:14])=[O:13]

参加物

4

反応物 2

HCID 84624-Chloro-alpha,alpha,alpha-trifluoro-3-nitrotolueneHCID 90863-Amino-1-propanol

生成物 1

HCID 28475091-Propanol, 3-[[2-nitro-4-(trifluoromethyl)phenyl]amino]-収率 100%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

A mixture of 100 parts of 1-chloro-2-nitro-4-(trifluoromethyl)benzene, 90 parts of 3-amino-1-propanol and 200 parts of butanol is stirred and heated till reflux. Stirring at reflux is continued overnight. The reaction mixture is cooled and evaporated. Water is added to the residue and the whole is acidified with a hydrochloric acid solution. The product is extracted with methylbenzene. The extract is dried, filtered and evaporated. The solid residue is crystallized from petroleumether. The product is filtered off and dried, yielding 141 parts (100%) of 3-{[2-nitro-4-(trifluoromethyl)phenyl]amino}-1-propanol.

後処理

  1. temperatureheated
  2. temperaturetill reflux
  3. stirringStirring
  4. temperatureat reflux
  5. temperatureThe reaction mixture is cooled
  6. customevaporated
  7. additionWater is added to the residue
  8. extractionThe product is extracted with methylbenzene
  9. customThe extract is dried
  10. filtrationfiltered
  11. customevaporated
  12. customThe solid residue is crystallized from petroleumether
  13. filtrationThe product is filtered off
  14. customdried

出典と根拠

ORDレコード
ord-0fc569756f4846f6bd4dc3333afcf253
出典データセット
uspto-grants-1979_11
特許番号
US04175129

関連ノート

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