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

HRID 2071229

반응식

HRID 2071229 반응식
[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

참가 물질

4

반응물 2

HCID 1490896o-Tolyl thiosemicarbazideHCID 27742172-Bromoethylamine hydrobromide

생성물 1

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

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5cc81af0d93a4bf2a3a8be020684b154
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04046753

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