Carbon Disulfide → 5-Methyl-2-pyridyldithiocarbamic acid triethylamine salt

HRID 27903

反応式

HRID 27903 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][N:3]=1.[C:9](=[S:11])=[S:10].[CH2:12]([N:14]([CH2:17][CH3:18])[CH2:15][CH3:16])[CH3:13]>>[CH2:12]([N:14]([CH2:17][CH3:18])[CH2:15][CH3:16])[CH3:13].[CH3:8][C:5]1[CH:6]=[CH:7][C:2]([NH:1][C:9](=[S:10])[SH:11])=[N:3][CH:4]=1

参加物

4

反応物 3

HCID 6348Carbon DisulfideHCID 8471TriethylamineHCID 153482-Amino-5-methylpyridine

生成物 1

HCID 123832335-Methyl-2-pyridyldithiocarbamic acid triethylamine salt収率 66%

実験手順

2-Amino-5-methylpyridine (21.6 g., 0.2 mol.) was suspended in triethylamine (60 ml.) and carbon disulphide (30 ml.) was added. The mixture was shaken at room temperature for 3 hours. The pale yellow solid precipitate was filtered off and washed with ether to give 5-methyl-2-pyridyldithiocarbamic acid triethylamine salt (37.7 g., 66%). This material was suspended in ethanol (100 ml.) and stirred at room temperature. Benzyl chloride (16.5 g., 15 ml.) was added dropwise. After 2 hours, a clear solution was obtained. Water was added and the precipitated benzyl ester collected. After washing with water and petrol ether (40°-60° C.), the product weighed 33.8 g. (m.pt. 141° C.).

後処理

  1. filtrationThe pale yellow solid precipitate was filtered off
  2. washwashed with ether

出典と根拠

ORDレコード
ord-03f468ff2c5248cb87bc911bddfce83c
出典データセット
uspto-grants-1980_09
特許番号
US04224331

関連ノート

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