Lithium Hydroxide → HCID 86669558、化合物

HRID 524433ノート

反応式

HRID 524433 の反応式
[CH:1]1([S:4]([C:7]2[CH:12]=[CH:11][C:10]([CH:13]([O:34][C@@H:35]3[CH2:39][CH2:38][O:37][CH2:36]3)[C:14]([NH:16][C:17]3[S:18][C:19]([O:22][C:23]4[CH:24]=[CH:25][C:26]([CH3:33])=[C:27]([CH:32]=4)[C:28]([O:30]C)=[O:29])=[CH:20][N:21]=3)=[O:15])=[CH:9][CH:8]=2)(=[O:6])=[O:5])[CH2:3][CH2:2]1.[Li+].[OH-]>C1COCC1.CO>[CH:1]1([S:4]([C:7]2[CH:12]=[CH:11][C:10]([CH:13]([O:34][C@@H:35]3[CH2:39][CH2:38][O:37][CH2:36]3)[C:14]([NH:16][C:17]3[S:18][C:19]([O:22][C:23]4[CH:24]=[CH:25][C:26]([CH3:33])=[C:27]([CH:32]=4)[C:28]([OH:30])=[O:29])=[CH:20][N:21]=3)=[O:15])=[CH:9][CH:8]=2)(=[O:6])=[O:5])[CH2:2][CH2:3]1

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 86669552HCID 86669552、化合物

生成物 1

HCID 86669558HCID 86669558、化合物収率 88.8%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

5-[2-[[2-(4-cyclopropylsulfonylphenyl)-2-[(3R)-tetrahydrofuran-3-yl]oxy-acetyl]amino]thiazol-5-yl]oxy-2-methyl-benzoic acid methyl ester (Example A3; 0.300 g, 0.524 mmol) was taken in THF(4 mL) and MeOH (0.1 mL), to it was added aqueous solution of LiOH (0.110 g, 2.62 mmol in 7 mL water) and stirred for 1-4 h at room temperature. After completion of the reaction, organic solvent was removed under reduced pressure. The aqueous layer was washed with diisopropyl ether then acidified with 1 N HCl to pH 2. The solid formed was filtered, washed with water, followed by washing with diisopropyl ether & dried under vacuum to get the title compound (0.260 g).

後処理

  1. customAfter completion of the reaction, organic solvent
  2. customwas removed under reduced pressure
  3. washThe aqueous layer was washed with diisopropyl ether
  4. customThe solid formed
  5. filtrationwas filtered
  6. washwashed with water
  7. washby washing with diisopropyl ether
  8. customdried under vacuum

出典と根拠

ORDレコード
ord-c6d7a78d83bb46ebbc685ce330c95415
出典データセット
uspto-grants-2016_05
特許番号
US09340506B2

反応ノート

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