Thiocyanate → 2-(3,4-Dichlorophenyl)-1-hydrazinecarbothioamide

HRID 1665203

反応式

HRID 1665203 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][NH2:10])[CH:5]=[CH:6][C:7]=1[Cl:8].[S-:11][C:12]#[N:13].[K]>O>[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][NH:10][C:12]([NH2:13])=[S:11])[CH:5]=[CH:6][C:7]=1[Cl:8]

参加物

5

反応物 3

HCID 9322ThiocyanateHCID 83161(3,4-Dichlorophenyl)hydrazineHCID 5462222Potassium

生成物 1

HCID 37596382-(3,4-Dichlorophenyl)-1-hydrazinecarbothioamide収率 95%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 3,4-dichlorophenylhydrazine (18.8 mmol) and thiocyanate of potassium (55.7 mmol) was dissolved in water (1 L) and heated for 17 hours. After cooling the product the solid was filtered and dried in vacuo to give 3,4-dichlorophenylthiosemicarbazide (4.20 g, yield=95%). H1NMR (300 MHz, DMSO, 25° C.) δ: 9.37 (s, 1H); 8.30 (s, 1H); 7.84 (s, 1H); 7.60 (s, 1H); 7.40 (d, J=8.7 Hz, 1H); 6.37 (d, J=2.52 Hz. 1H); 6.60 (dd, J=8.67 Hz, J=2.5 Hz. 1H) ppm. EM (ES+) m/z=236 (100%) [M+H]+.

後処理

  1. temperatureheated for 17 hours
  2. temperatureAfter cooling the product the solid
  3. filtrationwas filtered
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-744fab7376ab41578e64f65c2de4503b
出典データセット
uspto-grants-2011_10
特許番号
US08039497B2

関連ノート

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