Ethanol → HCID 178512100, 화합물

HRID 2419778

반응식

HRID 2419778 반응식
I.[Cl:2][C:3]1[CH:15]=[CH:14][CH:13]=[C:12]([Cl:16])[C:4]=1[CH:5]=[N:6][NH:7][C:8](=[NH:11])SC.[CH2:17]([NH2:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C(O)C>O>[CH2:17]([NH:24][C:8]([NH:7][N:6]=[CH:5][C:4]1[C:12]([Cl:16])=[CH:13][CH:14]=[CH:15][C:3]=1[Cl:2])=[NH:11])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

참가 물질

5

반응물 3

HCID 702EthanolHCID 7504BenzylamineHCID 178504060Methyl 3-(2,6-dichlorobenzylidene)thiocarbazimidate hydroiodide

생성물 1

HCID 178512100HCID 178512100, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 93.6 g of methyl 3-(2,6-dichlorobenzylidene)thiocarbazimidate hydroiodide (U.S. Pat. No. 3,657,337) and 51.2 of benzylamine in 400 ml. of absolute ethanol is heated at reflux for 6 hours and then diluted while hot with 400 ml. of water, causing the separation of an oil. On standing, the oil crystallizes and the nearly colorless crystals are recovered by filtration. Recrystallization from aqueous ethanol gives the desired product as pale yellow crystals, m.p. 134°-137° C.

후처리

  1. temperatureat reflux for 6 hours
  2. additiondiluted while hot with 400 ml
  3. customthe separation of an oil
  4. customthe oil crystallizes
  5. filtrationthe nearly colorless crystals are recovered by filtration
  6. customRecrystallization from aqueous ethanol

출처 및 근거

ORD 기록
ord-1d5415641c3a4837909b31b0e8f6a582
출처 데이터셋
uspto-grants-1978_08
특허 번호
US04107326

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