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

HRID 1665203

반응식

HRID 1665203 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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]+.

후처리

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

출처 및 근거

ORD 기록
ord-744fab7376ab41578e64f65c2de4503b
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08039497B2

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