o-Tolyl thiosemicarbazide → 2-(o-Tolylhydrazino)-2-Thiazoline

HRID 2071229

反応式

HRID 2071229 の反応式
[C:1]1([CH3:12])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][NH:8][C:9]([NH2:11])=[S:10].Br.Br[CH2:15][CH2:16]N>C(O)(C)C>[C:1]1([CH3:12])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][NH:8][C:9]1[S:10][CH2:15][CH2:16][N:11]=1

参加物

4

反応物 2

HCID 1490896o-Tolyl thiosemicarbazideHCID 27742172-Bromoethylamine hydrobromide

生成物 1

HCID 124050132-(o-Tolylhydrazino)-2-Thiazoline

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A mixture of 27.2 g. (0.15 moles) of 1-(o-tolyl)-3-thiosemicarbazide, 31 g. (0.15 moles) of 2-bromoethylamine hydrobromide, and 800 ml. of isopropanol are heated at reflux temperature for 16 hours. The reaction mixture is cooled to room temperature and filtered. The solid material is washed with hot water and the aqueous solution is treated with saturated sodium bicarbonate solution. The solid material which separates is filtered, washed with water, and recrystallized with methanol affording 13 g. of 2-(o-tolylhydrazino)-2-thiazoline, m.p. 126°-127° C.

後処理

  1. additionA mixture of 27.2 g
  2. temperatureat reflux temperature for 16 hours
  3. filtrationfiltered
  4. washThe solid material is washed with hot water
  5. additionthe aqueous solution is treated with saturated sodium bicarbonate solution
  6. filtrationThe solid material which separates is filtered
  7. washwashed with water
  8. customrecrystallized with methanol affording 13 g

出典と根拠

ORDレコード
ord-5cc81af0d93a4bf2a3a8be020684b154
出典データセット
uspto-grants-1977_09
特許番号
US04046753

関連ノート

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