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Hydrochloric Acid → HCID 11433023, 화합물

HRID 732230
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인쇄 미리보기

반응식

HRID 732230 반응식
[F:1][CH:2]([CH2:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([CH2:23][N:24]([CH2:36][CH2:37][C:38]3[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=3)[C:25]3[S:26][CH:27]=[C:28]([C:30]4[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=4)[N:29]=3)=[CH:19][CH:18]=2)=[CH:11][CH:10]=1)[C:3]([O:5]CC)=[O:4].O1CCCC1.O.[OH-].[Li+].Cl>O.CO>[F:1][CH:2]([CH2:8][C:9]1[CH:10]=[CH:11][C:12]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([CH2:23][N:24]([CH2:36][CH2:37][C:38]3[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=3)[C:25]3[S:26][CH:27]=[C:28]([C:30]4[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=4)[N:29]=3)=[CH:19][CH:18]=2)=[CH:13][CH:14]=1)[C:3]([OH:5])=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 168937Lithium hydroxide, monohydrateHCID 23143237HCID 23143237, 화합물

생성물 1

HCID 11433023HCID 11433023, 화합물수율 68%

시약·촉매·용매 2

HCID 887Methanol용매
HCID 962
Water
용매

실험 절차

A mixture of ethyl 2-fluoro-3-{4-[(4-{[(2-phenylethyl)(4-phenyl-1,3-thiazol-2-yl)amino]methyl}benzyl)oxy]phenyl}-propanoate (740 mg, 1.31 mmol), tetrahydrofuran (15 mL), methanol (10 mL), water (10 mL) and lithium hydroxide monohydrate (165 mg, 3.92 mmol) was stirred at room temperature for 3 hr. The reaction mixture was neutralized with 1N hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was recrystallized from hexane-diisopropyl ether to give the title compound (505 mg, yield 68%) as colorless crystals.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customThe residue was recrystallized from hexane-diisopropyl ether

출처 및 근거

ORD 기록
ord-8dd78c1699cc4c39b1fe95fae90979ca
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07585880B2

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