Sodium hydride → Oxadixyl

HRID 67905ノート

反応式

HRID 67905 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 53735Oxadixyl

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-fffd76d46a214db79031677a4bdceb18
出典データセット
uspto-grants-1982_08
特許番号
US04347253

反応ノート

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