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Ethanol → HCID 20506266、化合物

HRID 354942
ノート
印刷プレビュー

反応式

HRID 354942 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[NH:9][CH2:10][CH2:11][CH2:12][OH:13].O[CH:15]([CH:20]1[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1)S([O-])(=O)=O.[Na+].C(O)C>O>[Cl:8][C:5]1[CH:6]=[CH:7][C:2]2[N:1]=[C:15]([CH:20]3[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]3)[N:9]([CH2:10][CH2:11][CH2:12][OH:13])[C:3]=2[CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 702EthanolHCID 20506299HCID 20506299、化合物HCID 24965326Cyclohexanemethanesulfonic acid, α-hydroxy-, sodium salt (1:1)

生成物 1

HCID 20506266HCID 20506266、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 40 parts of 3-[(2-amino-5-chlorophenyl)amino]-1-propanol, 87 parts of sodium α-hydroxycyclohexanemethanesulfonate and 200 parts of ethanol is stirred and refluxed for 10 minutes. The reaction mixture is diluted with water and the solvent is evaporated. The residue is extracted a few times with trichloromethane. The combined extracts are dried, filtered and evaporated. The oily residue is triturated in 2,2'-oxybispropane: a sticky tar precipitates. The 2,2'-oxybispropane is decanted and upon stirring at room temperature, the product is allowed to precipitate. It is filtered off and dried, yielding 6-chloro-2-cyclohexyl-1H-benzimidazole-1-propanol; mp. 120.1° C.

後処理

  1. temperaturerefluxed for 10 minutes
  2. customthe solvent is evaporated
  3. extractionThe residue is extracted a few times with trichloromethane
  4. customThe combined extracts are dried
  5. filtrationfiltered
  6. customevaporated
  7. customThe oily residue is triturated in 2,2'-oxybispropane
  8. customa sticky tar precipitates
  9. customThe 2,2'-oxybispropane is decanted
  10. stirringupon stirring at room temperature
  11. customto precipitate
  12. filtrationIt is filtered off
  13. customdried

出典と根拠

ORDレコード
ord-eabe7a3bb4d14ef59448f090fbe19e70
出典データセット
uspto-grants-1983_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04377578

反応ノート

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