Lithium Hydroxide → HCID 67354275, 화합물

HRID 75814노트

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HRID 75814 반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10](=[O:34])[NH:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]2[N:22]=[C:21]([C:23]([NH:25][CH:26]([CH:31]([CH3:33])[CH3:32])[C:27]([O:29]C)=[O:28])=[O:24])[O:20][N:19]=2)=[CH:14][CH:13]=1.[OH-].[Li+]>C1COCC1>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10](=[O:34])[NH:11][C:12]1[CH:13]=[CH:14][C:15]([C:18]2[N:22]=[C:21]([C:23]([NH:25][CH:26]([CH:31]([CH3:32])[CH3:33])[C:27]([OH:29])=[O:28])=[O:24])[O:20][N:19]=2)=[CH:16][CH:17]=1

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 67354586Methyl 2-(3-(4-(3-(2,4-difluorophenyl) ureido)phenyl)-1,2,4-oxadiazole-5-carboxamido)-3-methylbutanoate

생성물 1

HCID 67354275HCID 67354275, 화합물수율 81.89%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Methyl 2-(3-(4-(3-(2,4-difluorophenyl) ureido)phenyl)-1,2,4-oxadiazole-5-carboxamido)-3-methylbutanoate was added to THF and to this 1N lithium hydroxide was added and stirred at room temperature. After completion of the reaction the solvent was evaporated and the crude product so obtained was dissolved in ethyl acetate and washed with water, brine, dried by sodium sulphate and concentrated to give a solid. The solid was then purified by column chromatography. Yield 81.89%; 1H NMR (DMSO-d6) δ: 0.96 (d, 6H, C(CH3)2), 2.20 (m, 1H, CHMe2), 4.231 (m, 1H, NHCH), 7.07 (m, 1H), 7.35 (m, 1H), 7.67 (d, 2H), 8.011 (d, 2H), 8.10 (m, 1H), 8.61 (s, 1H, NH), 9.372 (s, 1H, NH), 9.39 (s, 1H, NH), 13.025 (s, 1H, COOH); MS (m/z) 458 (M+−1).

후처리

  1. additionwas added
  2. customAfter completion of the reaction the solvent
  3. customwas evaporated

출처 및 근거

ORD 기록
ord-c32e882608754b5a8435d15b5c02518c
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835428B2

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