Hydrochloric Acid → 3-Hydroxy-4-cyclohexylphenylglyoxylic acid

HRID 426795

反応式

HRID 426795 の反応式
N[C:2]1[CH:3]=[C:4]([C:14](=[O:20])[C:15]([O:17]CC)=[O:16])[CH:5]=[CH:6][C:7]=1[CH:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1.Cl.N([O-])=[O:23].[Na+]>O>[OH:23][C:2]1[CH:3]=[C:4]([C:14](=[O:20])[C:15]([OH:17])=[O:16])[CH:5]=[CH:6][C:7]=1[CH:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1

参加物

5

反応物 3

HCID 313Hydrochloric Acid2 回HCID 20515218Ethyl 3-amino-4-cyclohexylphenylglyoxylateHCID 23668193Sodium Nitrite

生成物 1

HCID 205151473-Hydroxy-4-cyclohexylphenylglyoxylic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 4.5 g. of ethyl 3-amino-4-cyclohexylphenylglyoxylate suspension in 125 ml. of 80% hydrochloric acid and cooled to 0° C. is added dropwise a solution of 1.2 g. of sodium nitrite in 15 ml. of water. After about 10 min., 200 ml. of 50% hydrochloric acid is added portion wise and stirred for 15 hours. The reaction mixture is then poured onto ice water and extracted with chloroform, dried over sodium sulfate and concentrated in vacuo. The residue is crystallized to obtain 3-hydroxy-4-cyclohexylphenylglyoxylic acid.

後処理

  1. additionis added dropwise a solution of 1.2 g
  2. additionThe reaction mixture is then poured onto ice water
  3. extractionextracted with chloroform
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe residue is crystallized

出典と根拠

ORDレコード
ord-0463b1133d1140faa46489f6cfbc4436
出典データセット
uspto-grants-1979_10
特許番号
US04171373

関連ノート

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