Sodium hydride → Oxadixyl

HRID 67905노트

반응식

HRID 67905 반응식
[CH3:1][O:2][CH2:3][C:4]([N:6]([C:14]1[C:19]([CH3:20])=[CH:18][CH:17]=[CH:16][C:15]=1[CH3:21])[NH:7][C:8]([O:10][CH2:11][CH2:12]Cl)=[O:9])=[O:5].[H-].[Na+]>C1(C)C=CC=CC=1>[CH3:1][O:2][CH2:3][C:4]([N:6]([C:14]1[C:19]([CH3:20])=[CH:18][CH:17]=[CH:16][C:15]=1[CH3:21])[N:7]1[CH2:12][CH2:11][O:10][C:8]1=[O:9])=[O:5]

참가 물질

4

반응물 2

HCID 24758Sodium hydrideHCID 204544942-Chloroethyl 2-(methoxyacetyl)-2-(2,6-dimethylphenyl)-hydrazinecarboxylate

생성물 1

HCID 53735Oxadixyl

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

11.8 g (0.0375 mol) 2-Chloroethyl 2-(methoxyacetyl)-2-(2,6-dimethylphenyl)-hydrazinecarboxylate are added portion-wise to a suspension of 2.0 g sodium hydride (in form of about 55% by weight in mineral oil) in 100 ml absolute toluene at room temperature under a blanket of nitrogen. The reaction temperature rises gradually during this addition up to 40°. After the addition is complete the mixture is stirred during 30 minutes without cooling and afterwards cooled to 10°. The unreacted sodium hydride is then destroyed with ethanol, the obtained solution washed with water dried with MgSO4 and the solvent removed in vacuo to give the end title compound which is recrystallised from ethanol to yield the title compound as colourless crystals. m.p. 103°-104°.

후처리

  1. additionThe reaction temperature rises gradually during this addition up to 40°
  2. additionAfter the addition
  3. temperaturewithout cooling
  4. temperatureafterwards cooled to 10°
  5. customThe unreacted sodium hydride is then destroyed with ethanol
  6. washthe obtained solution washed with water
  7. dry with materialdried with MgSO4
  8. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-fffd76d46a214db79031677a4bdceb18
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04347253

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