Lithium Hydroxide → HCID 68512729, 화합물

HRID 508124노트

반응식

HRID 508124 반응식
C[O:2][C:3](=[O:35])[CH2:4][NH:5][C:6]([C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]([C:18]2[CH2:22][C:21]([C:27]3[CH:32]=[C:31]([Cl:33])[CH:30]=[C:29]([Cl:34])[CH:28]=3)([C:23]([F:26])([F:25])[F:24])[O:20][N:19]=2)=[CH:10][CH:9]=1)=[O:7].[OH-].[Li+]>O1CCCC1.O>[Cl:34][C:29]1[CH:28]=[C:27]([C:21]2([C:23]([F:25])([F:24])[F:26])[O:20][N:19]=[C:18]([C:11]3[C:12]4[C:17](=[CH:16][CH:15]=[CH:14][CH:13]=4)[C:8]([C:6]([NH:5][CH2:4][C:3]([OH:35])=[O:2])=[O:7])=[CH:9][CH:10]=3)[CH2:22]2)[CH:32]=[C:31]([Cl:33])[CH:30]=1

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 68514950HCID 68514950, 화합물2회

생성물 1

HCID 68512729HCID 68512729, 화합물수율 99%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of N—[[4-[5-(3,5-dichlorophenyl)-4,5-dihydro-5-(trifluoromethyl)-3-isoxazolyl]-1-naphthalenyl]carbonyl]glycine methyl ester (i.e. the title product of Step A) (620 mg) in tetrahydrofuran (5 mL) was added an aqueous solution of lithium hydroxide (300 mg in 5 mL of water). After stirring at room temperature for 1 h, the reaction mixture was diluted with water and extracted with hexane. The aqueous layer was acidified with 6.0 N HCl to pH=2, causing a white precipitate to form. The aqueous mixture was extracted with ethyl acetate, washed with brine, dried with anhydrous sodium sulfate, and concentrated to afford the title compound as a white solid (600 mg, 99% yield).

후처리

  1. extractionextracted with hexane
  2. customto form
  3. extractionThe aqueous mixture was extracted with ethyl acetate
  4. washwashed with brine
  5. dry with materialdried with anhydrous sodium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e83acbad591142879f4f6c24840061e9
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09095138B2

반응 노트

불러오는 중…