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

HRID 365000ノート

反応式

HRID 365000 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-db9cecb607904804810b09c151d26606
出典データセット
uspto-grants-1986_08
特許番号
US04607107

反応ノート

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