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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Lithium hydroxide, monohydrate → HCID 59377707、化合物

HRID 1691792
ノート
印刷プレビュー

反応式

HRID 1691792 の反応式
C([O:3][C:4](=[O:25])[CH2:5][C:6]1[CH:11]=[C:10]([O:12][CH2:13][CH2:14][O:15][Si:16]([C:19]([CH3:22])([CH3:21])[CH3:20])([CH3:18])[CH3:17])[C:9]([F:23])=[CH:8][C:7]=1[Br:24])C.O[Li].O>CO>[Br:24][C:7]1[CH:8]=[C:9]([F:23])[C:10]([O:12][CH2:13][CH2:14][O:15][Si:16]([C:19]([CH3:20])([CH3:22])[CH3:21])([CH3:17])[CH3:18])=[CH:11][C:6]=1[CH2:5][C:4]([OH:25])=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 59377706HCID 59377706、化合物

生成物 1

HCID 59377707HCID 59377707、化合物収率 74.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of {2-bromo-5-[2-(tert-butyl-dimethyl-silanyloxy)-ethoxy]-4-fluoro-phenyl}-acetic acid ethyl ester (0.508 g, 1.16 mmol) in MeOH was added LiOH.H2O (0.036 g, 1.51 mmol). The mixture was stirred at room temperature for two hours, and then solvent was removed under reduced pressure. 2N NaOH was added to the residue, and the mixture was washed with diethyl ether. The aqueous phase was taken to pH 1 with 2N HCl and was extracted with EtOAc. The combined EtOAc extracts were washed with water, brine dried over MgSO4, filtered and concentrated to dryness under reduced pressure to yield {2-bromo-5-[2-(tert-butyl-dimethyl-silanyloxy)-ethoxy]-4-fluoro-phenyl}-acetic acid (0.352 g, 74%) as a white solid.

後処理

  1. customsolvent was removed under reduced pressure
  2. addition2N NaOH was added to the residue
  3. washthe mixture was washed with diethyl ether
  4. extractionwas extracted with EtOAc
  5. washThe combined EtOAc extracts were washed with water, brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-f779c62c4ebd4d81a8c8ead75cb675b6
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08153808B2

反応ノート

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