Hydrochloric Acid → HCID 58575185、化合物

HRID 1189456ノート

反応式

HRID 1189456 の反応式
C([NH:5][C:6]1[C:15]([N+:16]([O-:18])=[O:17])=[CH:14][C:9]([C:10]([O:12][CH3:13])=[O:11])=[C:8]([CH2:19][O:20][CH3:21])[CH:7]=1)(C)(C)C.Cl>CO>[NH2:5][C:6]1[C:15]([N+:16]([O-:18])=[O:17])=[CH:14][C:9]([C:10]([O:12][CH3:13])=[O:11])=[C:8]([CH2:19][O:20][CH3:21])[CH:7]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 67134197HCID 67134197、化合物

生成物 1

HCID 58575185HCID 58575185、化合物収率 85.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a mixed liquid of 6.80 g of methyl 4-(tert-butylamino)-2-(methoxymethyl)-5-nitrobenzoate and 68.0 mL of methanol was added 37.0 mL of 6 M hydrochloric acid, followed by stirring overnight under the heating and refluxing condition. The solvent was evaporated under reduced pressure, and then 111 mL of methanol and 1.00 mL of concentrated sulfuric acid were added thereto, followed by stirring overnight under the heating and refluxing condition. Ethyl acetate and a saturated aqueous sodium hydrogen carbonate solution were added thereto, followed by extraction with ethyl acetate, the organic layer was washed with saturated brine and then dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to obtain 4.73 g of methyl 4-amino-2-(methoxymethyl)-5-nitrobenzoate as a yellow solid.

後処理

  1. temperaturerefluxing condition
  2. customThe solvent was evaporated under reduced pressure
  3. addition111 mL of methanol and 1.00 mL of concentrated sulfuric acid were added
  4. stirringby stirring overnight under the heating and
  5. temperaturerefluxing condition
  6. additionEthyl acetate and a saturated aqueous sodium hydrogen carbonate solution were added
  7. extractionfollowed by extraction with ethyl acetate
  8. washthe organic layer was washed with saturated brine
  9. dry with materialdried over anhydrous magnesium sulfate
  10. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-4eeed101491746a6b8e333ed13332859
出典データセット
uspto-grants-2014_03
特許番号
US08674096B2

反応ノート

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