Lithium Hydroxide → HCID 68512729、化合物

HRID 467589ノート

反応式

HRID 467589 の反応式
C[O:2][C:3](=[O:35])[CH2:4][NH:5][C:6]([C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]([C:18]2[CH2:22][C:21]([C:27]3[CH:32]=[C:31]([Cl:33])[CH:30]=[C:29]([Cl:34])[CH:28]=3)([C:23]([F:26])([F:25])[F:24])[O:20][N:19]=2)=[CH:10][CH:9]=1)=[O:7].[OH-].[Li+]>O1CCCC1.O>[Cl:34][C:29]1[CH:28]=[C:27]([C:21]2([C:23]([F:25])([F:24])[F:26])[O:20][N:19]=[C:18]([C:11]3[C:12]4[C:17](=[CH:16][CH:15]=[CH:14][CH:13]=4)[C:8]([C:6]([NH:5][CH2:4][C:3]([OH:35])=[O:2])=[O:7])=[CH:9][CH:10]=3)[CH2:22]2)[CH:32]=[C:31]([Cl:33])[CH:30]=1

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 68514950HCID 68514950、化合物2 回

生成物 1

HCID 68512729HCID 68512729、化合物収率 99%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of N-[[4-[5-(3,5-dichlorophenyl)-4,5-dihydro-5-(trifluoromethyl)-3-isoxazolyl]-1-naphthalenyl]carbonyl]glycine methyl ester (i.e. the title product of Step A) (620 mg) in tetrahydrofuran (5 mL) was added an aqueous solution of lithium hydroxide (300 mg in 5 mL of water). After stirring at room temperature for 1 h, the reaction mixture was diluted with water and extracted with hexane. The aqueous layer was acidified with 6.0 N HCl to pH=2, causing a white precipitate to form. The aqueous mixture was extracted with ethyl acetate, washed with brine, dried with anhydrous sodium sulfate, and concentrated to afford the title compound as a white solid (600 mg, 99% yield).

後処理

  1. extractionextracted with hexane
  2. customto form
  3. extractionThe aqueous mixture was extracted with ethyl acetate
  4. washwashed with brine
  5. dry with materialdried with anhydrous sodium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-722263ee1f8944fb8dbba2c2af6732db
出典データセット
uspto-grants-2014_01
特許番号
US08623875B2

反応ノート

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