Benzylamine → HCID 178512100、化合物

HRID 2419779ノート

反応式

HRID 2419779 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>[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

4

反応物 2

HCID 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 702Ethanol溶媒

実験手順

A solution of 11.7 g. of methyl 3-(2,6-dichlorobenzylidene)thiocarbazimidate hydroiodide (U.S. Pat. No. 3,657,337) and 3.37 g. of benzylamine in 25 ml. of ethanol is heated at reflux for 18 hours and then evaporated to dryness under reduced pressure. The residue is partitioned between 80 ml. of diethyl ether and 100 ml. of water and the aqueous extract is made alkaline with ammonia. A pale yellow solid is recovered by filtration and recrystallized from aqueous ethanol, giving the desired product as colorless crystals, m.p. 133°-135° C.

後処理

  1. temperatureat reflux for 18 hours
  2. customevaporated to dryness under reduced pressure
  3. customThe residue is partitioned between 80 ml
  4. extractionof water and the aqueous extract
  5. filtrationA pale yellow solid is recovered by filtration
  6. customrecrystallized from aqueous ethanol

出典と根拠

ORDレコード
ord-1407a14b899c4749a1a15926ffc3de7e
出典データセット
uspto-grants-1978_08
特許番号
US04107326

反応ノート

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