Water → HCID 178503587、化合物

HRID 2164534ノート

反応式

HRID 2164534 の反応式
Cl.[CH3:2][CH:3]([CH3:7])[C:4](=[NH:6])[NH2:5].[H-].[Na+].[C:10]([C:12](=[C:17](SC)[S:18][CH3:19])[C:13](OC)=[O:14])#[N:11].O>CN(C)C=O>[CH3:2][CH:3]([C:4]1[NH:6][C:17]([S:18][CH3:19])=[C:12]([C:10]#[N:11])[C:13](=[O:14])[N:5]=1)[CH3:7]

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 319957Methyl 2-cyano-3,3-bis(methylsulfanyl)prop-2-enoateHCID 27820532-Methylpropanimidamide hydrochloride

生成物 1

HCID 178503587HCID 178503587、化合物収率 89.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒3 回

反応条件

温度
25 °C

実験手順

A solution of 2-methylpropanimidamide hydrochloride (7.0 g, described in Example 7) in dimethylformamide (15 mL) was added dropwise to a suspension of sodium hydride (3.0 g, 50% in mineral oil, prewashed with hexane) in dimethylformamide (15 mL) and the whole mixture was left at 25° C. for 1 hr. 2-Cyano-3,3-bis(methylthio)-2-propenoic acid, methyl ester (6.5 g) in dimethylformamide (15 mL) was then added dropwise, and the reaction mixture was stirred for an additional 4 hr at 25° C. Water (25 mL) was then added, and acidification with concentrated hydrochloric acid (10 mL) precipitated the product. The precipitate was collected and air dried to give the title compound (6.0 g): mp>260° C.

後処理

  1. customacidification with concentrated hydrochloric acid (10 mL) precipitated the product
  2. customThe precipitate was collected
  3. customair dried

出典と根拠

ORDレコード
ord-76a9c31ad9f24d1c811245ad555a643c
出典データセット
uspto-grants-1985_03
特許番号
US04505910

反応ノート

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