Ethanol → Ethyl 3-amino-2-nitrobenzoate

HRID 276026ノート

反応式

HRID 276026 の反応式
C([NH:4][C:5]1[C:6]([N+:14]([O-:16])=[O:15])=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([OH:10])=[O:9])(=O)C.S(=O)(=O)(O)O.[CH2:22](O)[CH3:23]>>[NH2:4][C:5]1[C:6]([N+:14]([O-:16])=[O:15])=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([O:10][CH2:22][CH3:23])=[O:9]

参加物

4

反応物 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 2932863-Acetamido-2-nitrobenzoic acid

生成物 1

HCID 18315537Ethyl 3-amino-2-nitrobenzoate

実験手順

A mixture of 20.2 of 3-acetylamino-2-nitrobenzoic acid, 11.4 g of 97% sulfuric acid and 300 ml of ethanol was stirred for 23 hours while being heat-refluxed. One-hundred milliliters of ethanol were distilled off under reduced pressure, and the residue was cooled to room temperature. Subsequently, the reaction solution was poured into 200 ml of ice water containing 19.5 g of sodium hydrogencarbonate. The crystals precipitated were separated through filtration, and were washed with water. Further, these crystals were dispersed in 30 ml of a mixed solution of ethyl acetate and hexane at a ratio of 1:2. The crystals were separated through filtration, washed with hexane, and then dried to give 18.0 g of ethyl 3-amino-2-nitrobenzoate.

後処理

  1. temperaturewhile being heat-refluxed
  2. distillationOne-hundred milliliters of ethanol were distilled off under reduced pressure
  3. additionSubsequently, the reaction solution was poured into 200 ml of ice water containing 19.5 g of sodium hydrogencarbonate
  4. customThe crystals precipitated
  5. customwere separated through filtration
  6. washwere washed with water
  7. additionFurther, these crystals were dispersed in 30 ml of a mixed solution of ethyl acetate and hexane at a ratio of 1:2
  8. customThe crystals were separated through filtration
  9. washwashed with hexane
  10. customdried

出典と根拠

ORDレコード
ord-b5e14b2d5ca14f708cfb78a626e0913b
出典データセット
uspto-grants-2002_03
特許番号
US06352985B1

反応ノート

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