Thiosemicarbazide → 3-Formylbenzamidine-thiosemicarbazone hydrochloride

HRID 1073844노트

반응식

HRID 1073844 반응식
[ClH:1].[CH:2]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[C:7]([NH2:9])=[NH:8])=O.[NH2:13][NH:14][C:15]([NH2:17])=[S:16]>CO.O.Cl>[ClH:1].[CH:2](=[N:13][NH:14][C:15]([NH2:17])=[S:16])[C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[C:7]([NH2:9])=[NH:8]

참가 물질

6

반응물 2

HCID 2723789ThiosemicarbazideHCID 27592083-Formylbenzamidine hydrochloride

생성물 1

HCID 867443493-Formylbenzamidine-thiosemicarbazone hydrochloride

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 887Methanol용매HCID 962Water용매2회

실험 절차

A solution of 1.84 g (~0.01 mol) of crude 3-formylbenzamidine hydrochloride (prepared analogously to Example 1b) in 10 ml of methanol is added dropwise to a solution of 0.91 g (0.01 mol) of thiosemicarbazide in 5 ml of water and 10 ml of 2N hydrochloric acid. This mixture is heated under reflux for 1 hour, cooled, filtered and concentrated to dryness by evaporation. The residue is recrystallised from methanol; m.p. 210° (with decomposition). The product contains 0.5 mol of water.

후처리

  1. temperatureThis mixture is heated
  2. temperatureunder reflux for 1 hour
  3. temperaturecooled
  4. filtrationfiltered
  5. concentrationconcentrated to dryness by evaporation
  6. customThe residue is recrystallised from methanol

출처 및 근거

ORD 기록
ord-a8dc2820b83c444f8aee7c1efb12984b
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04971986

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