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Lithium Hydroxide → HCID 18413994、化合物

HRID 991454
ノート
印刷プレビュー

反応式

HRID 991454 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

HCID 18413994HCID 18413994、化合物収率 100%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 962
Water
溶媒
2 回

実験手順

{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%).

後処理

  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

出典と根拠

ORDレコード
ord-438cf89834a5433d984fd49c1ae7848d
出典データセット
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06465468B1

反応ノート

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