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Methyl bromoacetate → HCID 54374596, 화합물

HRID 1493606
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HRID 1493606 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([NH:8][NH:9][C:10]([NH2:12])=[O:11])[CH:5]=[CH:6][CH:7]=1.Br[CH2:14][C:15]([O:17][CH3:18])=[O:16]>C1(C)C=CC=CC=1>[NH2:12][C:10]([NH:9][N:8]([CH2:14][C:15]([O:17][CH3:18])=[O:16])[C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([CH3:1])[CH:3]=1)=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 60984Methyl bromoacetateHCID 2396331-(m-Tolyl)semicarbazide

생성물 1

HCID 54374596HCID 54374596, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 2-(3-methylphenyl)hydrazinecarboxamide (5 g), DEA (10.5 ml) and methyl bromoacetate (4.5 ml) in toluene (100 ml) was heated under reflux for 20 h, and was then partitioned between ethyl acetate (200 ml) and water (200 ml). The organic layer was washed with water (2×100 ml) and saturated brine (100 ml) before being dried and evaporated in vacuo to leave an oil (6.1 g). This was purified by FCC eluting with ethyl acetate to give the title compound (4.4 g) as a solid, m.p. 68°-70° after recrystallisation from ethyl acetate and trituration with ether.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 20 h
  3. customwas then partitioned between ethyl acetate (200 ml) and water (200 ml)
  4. washThe organic layer was washed with water (2×100 ml) and saturated brine (100 ml)
  5. custombefore being dried
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-c71c63a4a3a84c258c9c3d1d6f7a188f
출처 데이터셋
uspto-grants-1991_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05023255

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