Hydrogen Bromide → 3-Bromo-4-cyclohexylphenylglyoxylic acid

HRID 26553

반응식

HRID 26553 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.[BrH:21].N([O-])=O.[Na+]>O>[Br:21][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 260Hydrogen Bromide2회HCID 20515218Ethyl 3-amino-4-cyclohexylphenylglyoxylateHCID 23668193Sodium Nitrite

생성물 1

HCID 205151793-Bromo-4-cyclohexylphenylglyoxylic acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 11.1 g. (0.044 moles) of ethyl 3-amino-4-cyclohexylphenylglyoxylate suspension in 225 ml. of 40% hydrobromic acid and cooled to 0° C. is added dropwise a solution of 2.34 g. of sodium nitrite in 30 ml. of water. To this mixture is added a solution of 20 g. of cuprous bromide in 350 ml. of 40% hydrobromic acid added portion wise and stirred for 15 hours. The reaction mixture is then poured onto ice water, extracted with chloroform, dried over sodium sulfate and concentrated in vacuo. The residue is then crystallized to obtain 3-bromo-4-cyclohexylphenylglyoxylic acid.

후처리

  1. additionis added dropwise a solution of 2.34 g
  2. additionTo this mixture is added a solution of 20 g
  3. additionThe reaction mixture is then poured onto ice water
  4. extractionextracted with chloroform
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue is then crystallized

출처 및 근거

ORD 기록
ord-bb566c1021da480894574cb6f8874be4
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04150148

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