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Cysteamine Hydrochloride → 2-[(4-Methyl-1,2,5-oxadiazol-3-yl)methylthio]ethylamine

HRID 1702280
ノート
印刷プレビュー

反応式

HRID 1702280 の反応式
O[CH2:2][C:3]1[C:7]([CH3:8])=[N:6][O:5][N:4]=1.Cl.[NH2:10][CH2:11][CH2:12][SH:13]>Br>[CH3:8][C:7]1[C:3]([CH2:2][S:13][CH2:12][CH2:11][NH2:10])=[N:4][O:5][N:6]=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 9082Cysteamine HydrochlorideHCID 1896971(4-Methyl-1,2,5-oxadiazol-3-yl)methanol

生成物 1

HCID 131028982-[(4-Methyl-1,2,5-oxadiazol-3-yl)methylthio]ethylamine

試薬・触媒・溶媒 1

HCID 260Hydrogen Bromide溶媒

実験手順

A solution of 3-hydroxymethyl-4-methylfurazan (2.49 g; 21.8 mmoles) [prepared in Step A] and 2-aminoethanethiol hydrochloride (2.48 g; 21.8 mmoles) in 60 ml of 48% aqueous hydrobromic acid was stirred and heated at reflux temperature for 23 hours and then at ambient temperature for 40 hours. The excess hydrobromic acid was removed under reduced pressure, and the oil residue was dissolved in isopropyl alcohol, filtered though Celite and the product was crystallized from the filtrate. Recrystallization from isopropyl alcohol yielded the title compound as the hydrobromide salt, mp 142°-143°.

後処理

  1. temperatureheated
  2. temperatureat reflux temperature for 23 hours
  3. customThe excess hydrobromic acid was removed under reduced pressure
  4. dissolutionthe oil residue was dissolved in isopropyl alcohol
  5. filtrationfiltered though Celite
  6. customthe product was crystallized from the filtrate
  7. customRecrystallization from isopropyl alcohol

出典と根拠

ORDレコード
ord-8054cb5cfffe43b694d1ab2fe427b9a7
出典データセット
uspto-grants-1983_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04380638

反応ノート

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