Lithium hydroxide, monohydrate → HCID 19077644, 화합물

HRID 1598794노트

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HRID 1598794 반응식
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]

참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 564797HCID 564797, 화합물

생성물 1

HCID 19077644HCID 19077644, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0b1fa790f30349059db6d7852fd895ac
출처 데이터셋
uspto-grants-1998_04
특허 번호
US05739160

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