Hydrochloric Acid → HCID 178485100、化合物

HRID 1283745

反応式

HRID 1283745 の反応式
[Cl:1][C:2]1[CH:8]=[CH:7][CH:6]=[C:5]([Cl:9])[C:3]=1[NH2:4].Cl.C1C(O)=CC=CC=1C.[CH3:19][NH:20][C:21]#[N:22].[OH-].[Na+]>CCOCC>[ClH:1].[Cl:1][C:2]1[CH:8]=[CH:7][CH:6]=[C:5]([Cl:9])[C:3]=1[NH:4][C:21]([NH:20][CH3:19])=[NH:22]

参加物

7

反応物 5

HCID 313Hydrochloric Acid2 回HCID 342M-CresolHCID 118462,6-DichloroanilineHCID 14798Sodium HydroxideHCID 119415Methylcyanamide

生成物 1

HCID 178485100HCID 178485100、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

To 51 g (0.315 mole) of 2,6-dichloroaniline is added 0.4 mole of ethereal HCl and 200 ml of m-cresol. The mixture is then stirred and heated on a steam bath to drive off the ether and excess hydrogen chloride. To the resultant mixture is then added 17.7 g (0.315 mole) of methyl cyanamide then heated for 2 hours on a steam bath. The reaction mixture is then cooled, added to 150 ml of conc. sodium hydroxide solution, cooled and extracted with 2 liters of ether. The ether layer is washed with 2 × 1 liter of water, dried over sodium sulfate, charcoaled and evaporated. The residue is triturated with hexane and the precipitate is filtered off and washed with ether and dried to obtain 1-(2,6-dichlorophenyl)-3-methylguanidine hydrochloride.

後処理

  1. temperatureheated on a steam bath
  2. temperaturethen heated for 2 hours on a steam bath
  3. temperatureThe reaction mixture is then cooled
  4. temperaturecooled
  5. extractionextracted with 2 liters of ether
  6. washThe ether layer is washed with 2 × 1 liter of water
  7. dry with materialdried over sodium sulfate
  8. customevaporated
  9. customThe residue is triturated with hexane
  10. filtrationthe precipitate is filtered off
  11. washwashed with ether
  12. customdried

出典と根拠

ORDレコード
ord-9d930eb8d6e44bfca99a0c305539527e
出典データセット
uspto-grants-1976_08
特許番号
US03976643

関連ノート

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