Citric Acid → 4-(3-chlorophenyl)sulfonylbenzoic acid

HRID 401662노트

반응식

HRID 401662 반응식
C[O:2][C:3](=[O:20])[C:4]1[CH:9]=[CH:8][C:7]([S:10]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[CH:14]=2)(=[O:12])=[O:11])=[CH:6][CH:5]=1.[Li+].[OH-].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>C1COCC1.CO.O>[Cl:19][C:15]1[CH:14]=[C:13]([S:10]([C:7]2[CH:8]=[CH:9][C:4]([C:3]([OH:20])=[O:2])=[CH:5][CH:6]=2)(=[O:11])=[O:12])[CH:18]=[CH:17][CH:16]=1

참가 물질

5

반응물 3

HCID 311Citric AcidHCID 3939Lithium HydroxideHCID 59625905HCID 59625905, 화합물

생성물 1

HCID 3438084-(3-chlorophenyl)sulfonylbenzoic acid

시약·촉매·용매 1

HCID 21892291Methanol tetrahydrofuran water용매

실험 절차

A mixture of compound 31a (138 mg, 0.44 mmol) and LiOH (42 mg, 1.77 mmol) in THF/MeOH/H2O (2/2/2 mL) was stirred for 4 h. A 15% citric acid solution (10 mL) was added. The mixture was then extracted with EtOAc (3×). The combined organic extracts were washed with brine, dried over Na2SO4, filtered, and concentrated under reduced pressure. The resultant residue, compound 31b (130 mg) was dried under reduced pressure for 18 h and used without further purification.

후처리

  1. extractionThe mixture was then extracted with EtOAc (3×)
  2. washThe combined organic extracts were washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. dry with materialThe resultant residue, compound 31b (130 mg) was dried under reduced pressure for 18 h
  7. customused without further purification

출처 및 근거

ORD 기록
ord-f2765e1c09d64e038c0a71a433c1ec6b
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08741887B2

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