Hydrochloric Acid → HCID 22494951、化合物

HRID 1862594ノート

反応式

HRID 1862594 の反応式
[C:1]([C:3]1[CH:12]=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[C:5]([N+:13]([O-:15])=[O:14])[CH:4]=1)#[N:2].CO.[ClH:18]>C1COCC1>[Cl-:18].[N+:13]([C:5]1[CH:4]=[C:3]([CH:12]=[CH:11][C:6]=1[C:7]([O:9][CH3:10])=[O:8])[CH2:1][NH3+:2])([O-:15])=[O:14]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 11356202Methyl 4-cyano-2-nitrobenzoate

生成物 1

HCID 22494951HCID 22494951、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

700 ml of a 1 M BH3 solution in THF (0.7 mol) are metered in the course of one hour at 40-50° C. into a solution of 144 g (0.7 mol) of methyl 4-cyano-2-nitrobenzoate in 250 ml of THF and the mixture is subsequently refluxed for a further 1.5 hours. The reaction mixture is then treated with 600 ml of methanol saturated with hydrogen chloride gas, with ice-cooling, and refluxed for one hour. The mixture is concentrated completely under atmospheric pressure and reevaporated with 700 ml of methanol. The residue which remains is stirred with 500 ml of ethyl acetate and filtered, and the product is dried. This gives 115 g (67%) of 3-nitro-4-methoxycarbonylbenzyl-ammonium chloride of melting point 247-248° C.

後処理

  1. temperaturethe mixture is subsequently refluxed for a further 1.5 hours
  2. temperaturecooling
  3. temperaturerefluxed for one hour
  4. concentrationThe mixture is concentrated completely under atmospheric pressure
  5. customreevaporated with 700 ml of methanol
  6. filtrationfiltered
  7. customthe product is dried

出典と根拠

ORDレコード
ord-8afbc4dec7ff4ba1aad4e756a0be980f
出典データセット
uspto-grants-2003_03
特許番号
US06538150B2

反応ノート

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