(+-)-Methionine → 3'-Hydroxy-[1,1'-biphenyl]-3-carboxylic acid

HRID 377311

반응식

HRID 377311 반응식
C[O:2][C:3]1[CH:4]=[C:5]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([OH:17])=[O:16])[CH:10]=2)[CH:6]=[CH:7][CH:8]=1.NC(C(O)=O)CCSC>CS(O)(=O)=O.O>[OH:2][C:3]1[CH:4]=[C:5]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([OH:17])=[O:16])[CH:10]=2)[CH:6]=[CH:7][CH:8]=1

참가 물질

5

반응물 2

HCID 876(+-)-MethionineHCID 27595503'-Methoxy-biphenyl-3-carboxylic acid

생성물 1

HCID 27593013'-Hydroxy-[1,1'-biphenyl]-3-carboxylic acid수율 93.3%

시약·촉매·용매 2

HCID 962Water용매HCID 6395Methanesulfonic Acid용매

실험 절차

A suspension of 3'-methoxy-3-biphenylcarboxylic acid (4.1 g) and DL-methionine (26.7 g) in methanesulfonic acid (116 ml) was stirred at room temperature for 22 hours, diluted with water, and extracted three times with diethyl ether. The extracts were combined, washed with brine, dried over magnesium sulfate, and evaporated in vacuo. The residue was crystallized from n-hexane to afford 3'-hydroxy-3-biphenylcarboxylic acid (3.59 g) as a colorless powder.

후처리

  1. extractionextracted three times with diethyl ether
  2. washwashed with brine
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe residue was crystallized from n-hexane

출처 및 근거

ORD 기록
ord-912e2197e69c4bb7a28b8e9c6f6a6ac3
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06025375

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