Hydrochloric Acid → 3-Hydroxy-4-cyclohexylphenylglyoxylic acid

HRID 616739

반응식

HRID 616739 반응식
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

참가 물질

5

반응물 3

HCID 313Hydrochloric Acid2회HCID 20515218Ethyl 3-amino-4-cyclohexylphenylglyoxylateHCID 23668193Sodium Nitrite

생성물 1

HCID 205151473-Hydroxy-4-cyclohexylphenylglyoxylic acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-63a2b4ae6adf4979b7cdf57056cd7563
출처 데이터셋
uspto-grants-1978_02
특허 번호
US04075354

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