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Sodium Hydroxide → HCID 178460306、化合物

HRID 325525
ノート
印刷プレビュー

反応式

HRID 325525 の反応式
[ClH:1].[CH2:2]([O:5][NH2:6])[CH2:3][CH3:4].[OH-].[Na+].S(O)(O)(=O)=O.CS[C:16](=[NH:18])[NH2:17]>O>[ClH:1].[CH2:2]([O:5][NH:6][C:16]([NH2:18])=[NH:17])[CH2:3][CH3:4]
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 14798Sodium HydroxideHCID 752702-Methyl-2-thiopseudourea sulfateHCID 12283955O-propylhydroxylamine hydrochloride

生成物 1

HCID 178460306HCID 178460306、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 113.2 g. of propoxyamine hydrochloride in 200 ml. of ice cold water there is added 81.2 g. of 50% aqueous sodium hydroxide solution. The mixture is stirred for thirty minutes and 141.0 g. of S-methyl-2-thiopseudourea sulfate and 200 ml. of water are added. The mixture is stirred at room temperature for two hours and then heated to reflux for one hour. The mixture is treated with 81.2 g. of 50% aqueous sodium hydroxide filtered and evaporated in vacuo. The residue is slurried in 200 ml. of absolute ethanol, the suspension filtered and the filtrate evaporated to an oil. The crude oil is dissolved in 300 ml. of chloroform, the mixture is cooled and filtered to give a clear solution of the guanidine free base. The chloroform solution is made acidic with methanolic hydrogen chloride and then evaporated in vacuo to give propoxyguanidine hydrochloride as a clear viscous oil (m.p. of picrate 179°-80° C.).

後処理

  1. additionof ice cold water there is added 81.2 g
  2. stirringThe mixture is stirred at room temperature for two hours
  3. temperatureheated
  4. temperatureto reflux for one hour
  5. additionThe mixture is treated with 81.2 g
  6. filtrationof 50% aqueous sodium hydroxide filtered
  7. customevaporated in vacuo
  8. filtrationof absolute ethanol, the suspension filtered
  9. customthe filtrate evaporated to an oil
  10. dissolutionThe crude oil is dissolved in 300 ml
  11. temperatureof chloroform, the mixture is cooled
  12. filtrationfiltered

出典と根拠

ORDレコード
ord-7a8e1e9323ae4bf5b64c11f7737eee04
出典データセット
uspto-grants-1984_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04440949

反応ノート

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