Lithium hydroxide, monohydrate → HCID 19077644、化合物

HRID 1598794ノート

反応式

HRID 1598794 の反応式
O[Li].O.[CH:4](=[C:6]1[CH2:10][CH:9]([C:11]([O:13]CC)=[O:12])[CH:8]([C:16]([O:18]CC)=[O:17])[CH2:7]1)[CH3:5]>O.C1COCC1>[CH:4](=[C:6]1[CH2:10][CH:9]([C:11]([OH:13])=[O:12])[CH:8]([C:16]([OH:18])=[O:17])[CH2:7]1)[CH3:5]

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 564797HCID 564797、化合物

生成物 1

HCID 19077644HCID 19077644、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of LiOH.H2O (5.1 g, 120 mmol) in 130 ml of water is added dropwise at 0° C. to a solution of the compound from Example VIII (13.1 g, 54.5 mmol) in 70 ml of THF. The solution is stirred at room temperature for 20 h, the THF is stripped off in vacuo and the residue is extracted once with 40 ml of ether. The aqueous phase is brought to pH 2 with 10% strength hydrochloric acid and extracted three times with 200 ml of ethyl acetate each time. The combined ethyl acetate phases are dried over Na2SO4 and the solvent is stripped off in vacuo.

後処理

  1. extractionthe residue is extracted once with 40 ml of ether
  2. extractionextracted three times with 200 ml of ethyl acetate each time
  3. dry with materialThe combined ethyl acetate phases are dried over Na2SO4

出典と根拠

ORDレコード
ord-0b1fa790f30349059db6d7852fd895ac
出典データセット
uspto-grants-1998_04
特許番号
US05739160

反応ノート

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