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Lithium Hydroxide → HCID 18413994, 화합물

HRID 991454
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HRID 991454 반응식
C[O:2][C:3](=[O:34])[CH2:4][C:5]1[CH:10]=[C:9]([O:11][CH3:12])[C:8]([O:13][CH3:14])=[CH:7][C:6]=1[S:15]([N:18]1[CH2:23][CH2:22][N:21]([C:24]2[CH:29]=[CH:28][C:27]([C:30]([F:33])([F:32])[F:31])=[CH:26][N:25]=2)[CH2:20][CH2:19]1)(=[O:17])=[O:16].O1CCCC1.[OH-].[Li+]>CO.O>[CH3:14][O:13][C:8]1[C:9]([O:11][CH3:12])=[CH:10][C:5]([CH2:4][C:3]([OH:34])=[O:2])=[C:6]([S:15]([N:18]2[CH2:23][CH2:22][N:21]([C:24]3[CH:29]=[CH:28][C:27]([C:30]([F:31])([F:33])[F:32])=[CH:26][N:25]=3)[CH2:20][CH2:19]2)(=[O:16])=[O:17])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 4446657Methyl 2-(4,5-dimethoxy-2-((4-(5-(trifluoromethyl)(2-pyridyl))piperazinyl)sulfonyl)phenyl)acetate

생성물 1

HCID 18413994HCID 18413994, 화합물수율 100%

시약·촉매·용매 2

HCID 887Methanol용매
HCID 962
Water
용매
2회

실험 절차

{4,5-Dimethoxy-2-[4-(5-trifluoromethylpyridin-2-yl)piperazine-1-sulfonyl]phenyl}acetic acid methyl ester (0.3 g) was taken up in methanol (10 ml), tetrahydrofuran (10 ml) and water (10 ml). Lithium hydroxide (125 mg) was added and the reaction stirred at RT for 16 hrs. The reaction was diluted with water (10 ml), its volume reduced to one third in vacuo, and the reaction extracted with diethyl ether (3×15 ml). The aqueous layer was acidified to pH 4 with 2M hydrochloric acid and extracted with ethyl acetate (4×25 ml). The combined ethyl acetate extracts were washed with water (25 ml) and brine (25 ml) and dried over sodium sulphate. The solvent was removed in vacuo to yield the title compound as a white solid (291 mg, 100%).

후처리

  1. extractionthe reaction extracted with diethyl ether (3×15 ml)
  2. extractionextracted with ethyl acetate (4×25 ml)
  3. washThe combined ethyl acetate extracts were washed with water (25 ml) and brine (25 ml)
  4. dry with materialdried over sodium sulphate
  5. customThe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-438cf89834a5433d984fd49c1ae7848d
출처 데이터셋
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06465468B1

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