Ethyl 8-methoxy-5-nitrochroman-3-carboxylate → HCID 22464172、化合物

HRID 1274943ノート

反応式

HRID 1274943 の反応式
C([O:3][C:4]([CH:6]1[CH2:11][C:10]2[C:12]([N+:18]([O-:20])=[O:19])=[CH:13][CH:14]=[C:15]([O:16][CH3:17])[C:9]=2[O:8][CH2:7]1)=[O:5])C>C(O)C.[OH-].[Na+]>[CH3:17][O:16][C:15]1[C:9]2[O:8][CH2:7][CH:6]([C:4]([OH:5])=[O:3])[CH2:11][C:10]=2[C:12]([N+:18]([O-:20])=[O:19])=[CH:13][CH:14]=1

参加物

4

反応物 1

HCID 18739724Ethyl 8-methoxy-5-nitrochroman-3-carboxylate

生成物 1

HCID 22464172HCID 22464172、化合物収率 94%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

A mixture of 8-methoxy-5-nitro-3,4-dihydro-2H-1-benzopyran-3-carboxylic acid ethyl ester (5.8 g, 21 mmol) in ethanol (150 nL) and 2 M NaOH (15 mL) was heated to reflux for 30 min. The solvent was evaporated in vacuo the residue dissolved in water. Acidification to pH 2 and extraction with ethyl acetate followed by evaporation of the solvent in vacuo gave 4.9 g (94% yield) of the title compound: mp 181-183° C.; EIMS (70 eV) m/z (relative intensity) 253 (55, M+).

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 30 min
  3. customThe solvent was evaporated in vacuo the residue
  4. dissolutiondissolved in water
  5. extractionAcidification to pH 2 and extraction with ethyl acetate
  6. customfollowed by evaporation of the solvent in vacuo

出典と根拠

ORDレコード
ord-200970214d584046a0340c20ae42c579
出典データセット
uspto-grants-2000_12
特許番号
US06159972

反応ノート

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