Hydrochloric Acid → 2-(4-Dimethylaminomethyl-2-pyridylmethylthio)ethylamine

HRID 1904077ノート

反応式

HRID 1904077 の反応式
Cl.[NH2:2][CH2:3][CH2:4][SH:5].[O-]CC.[Na+].Cl.Cl.Cl[CH2:13][C:14]1[CH:19]=[C:18]([CH2:20][N:21]([CH3:23])[CH3:22])[CH:17]=[CH:16][N:15]=1.Cl>C(O)C.O>[CH3:22][N:21]([CH2:20][C:18]1[CH:17]=[CH:16][N:15]=[C:14]([CH2:13][S:5][CH2:4][CH2:3][NH2:2])[CH:19]=1)[CH3:23]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 9082Cysteamine HydrochlorideHCID 2723922Sodium ethoxideHCID 132926032-Chloromethyl-4-dimethylaminomethylpyridine dihydrochloride

生成物 1

HCID 132773272-(4-Dimethylaminomethyl-2-pyridylmethylthio)ethylamine収率 73.6%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

Cysteamine hydrochloride (3.75 g) was added to a stirred solution of sodium ethoxide (prepared from 2.83 g sodium) in ethanol (200 ml) and the mixture was cooled to less than 10°. 2-Chloromethyl-4-dimethylaminomethylpyridine dihydrochloride (7.3 g) was added portionwise and the solution was stirred for 1 hour. Water (200 ml) was added, the pH was adjusted to ca. 4 with hydrochloric acid and the volume was reduced to ca. 100 ml. The solution was extracted with chloroform, the aqueous phase was basified to pH 12 and extracted with chloroform to give 2-(4-dimethylaminomethyl-2-pyridylmethylthio)ethylamine (4.7 g) as an oil.

後処理

  1. temperaturethe mixture was cooled to less than 10°
  2. extractionThe solution was extracted with chloroform
  3. extractionextracted with chloroform

出典と根拠

ORDレコード
ord-e31a6b66a98548438f2e6b7ad937f186
出典データセット
uspto-grants-1984_03
特許番号
US04439609

反応ノート

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