Lithium Hydroxide → HCID 68512729、化合物

HRID 1958874ノート

反応式

HRID 1958874 の反応式
[Li+].[OH-].C[O:4][C:5](=[O:37])[CH2:6][NH:7][C:8]([C:10]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[C:13]([C:20]2[CH2:24][C:23]([C:29]3[CH:34]=[C:33]([Cl:35])[CH:32]=[C:31]([Cl:36])[CH:30]=3)([C:25]([F:28])([F:27])[F:26])[O:22][N:21]=2)=[CH:12][CH:11]=1)=[O:9]>O1CCCC1.O>[Cl:36][C:31]1[CH:30]=[C:29]([C:23]2([C:25]([F:27])([F:26])[F:28])[O:22][N:21]=[C:20]([C:13]3[C:14]4[C:19](=[CH:18][CH:17]=[CH:16][CH:15]=4)[C:10]([C:8]([NH:7][CH2:6][C:5]([OH:37])=[O:4])=[O:9])=[CH:11][CH:12]=3)[CH2:24]2)[CH:34]=[C:33]([Cl:35])[CH:32]=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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

An aqueous solution of LiOH (300 mg, in 5 mL of H2O) was added 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 product of Step C, 620 mg) in tetrahydrofuran (5 mL). 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, and a white precipitate formed. The aqueous mixture was extracted with ethyl acetate. The organic extract was washed with brine, dried over sodium sulfate, and concentrated under reduced pressure to provide the title compound (600 mg) as a white solid. 1H NMR (Me2S(O)-d6): δ 9.02 (t, 1H), 8.81 (d, 1H), 8.37 (d, 1H), 7.92 (d, 1H), 7.83 (t, 1H), 7.65-7.74 (m, 5H), 4.58 (d, 1H), 4.54 (d, 1H), 4.02 (d, 2H).

後処理

  1. extractionextracted with hexane
  2. customa white precipitate formed
  3. extractionThe aqueous mixture was extracted with ethyl acetate
  4. extractionThe organic extract
  5. washwas washed with brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-90a88703efd54ced8c90d93a0008339e
出典データセット
uspto-grants-2013_04
特許番号
US08410153B2

反応ノート

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