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Lithium Hydroxide → HCID 69226247, 화합물

HRID 2113904
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HRID 2113904 반응식
C[O:2][C:3](=[O:24])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([C:10]2[O:14][N:13]=[C:12]([C:15]3[CH:16]=[N:17][C:18]([N:21]([CH3:23])[CH3:22])=[CH:19][CH:20]=3)[N:11]=2)[CH:5]=1.[Li+].[OH-]>O1CCOCC1>[CH3:22][N:21]([CH3:23])[C:18]1[N:17]=[CH:16][C:15]([C:12]2[N:11]=[C:10]([C:6]3[CH:5]=[C:4]([CH:9]=[CH:8][CH:7]=3)[C:3]([OH:24])=[O:2])[O:14][N:13]=2)=[CH:20][CH:19]=1
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참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 69222561HCID 69222561, 화합물

생성물 1

HCID 69226247HCID 69226247, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

In a 250 ml round flask, 7.0 g (21.6 mmol) of 3-[3-(6-dimethylamino-pyridin-3-yl)-[1,2,4]oxadiazol-5-yl]-benzoic acid methyl ester is dissolved in 150 ml of dioxane and treated with 32.4 ml (1M, 32.4 mmol, 1.5 eq.) of aqueous LiOH solution. After 20 h, the solvent is removed under vacuo and the residue suspended in 300 ml H2O. The pH value is then adjusted to 2 by addition of 1M HCl-solution. The precipitate is stirred for 30 minutes, then filtered, washed with 0.1 M HCl-solution and with diethyl-ether and dried. This yields the title compound as light yellow solid. Mass spectrum: m/z (M+H)+: 311.0

후처리

  1. customthe solvent is removed under vacuo
  2. additionThe pH value is then adjusted to 2 by addition of 1M HCl-solution
  3. filtrationfiltered
  4. washwashed with 0.1 M HCl-solution and with diethyl-ether
  5. customdried

출처 및 근거

ORD 기록
ord-40ffbae258d949a5975eb9685c0cf10d
출처 데이터셋
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07432293B2

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