Ethanol → HCID 178512100、化合物

HRID 2419778

反応式

HRID 2419778 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 178512100HCID 178512100、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1d5415641c3a4837909b31b0e8f6a582
出典データセット
uspto-grants-1978_08
特許番号
US04107326

関連ノート

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