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Water → Tert-butyl 3-[6-chloro-2-(2,2-dimethylpropanamido)pyridin-3-yl]-3-hydroxypropanoate

HRID 1373583
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HRID 1373583 반응식
C[Si](C)(C)N[Si](C)(C)C.[Li].[C:11]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])(=[O:13])[CH3:12].[Cl:19][C:20]1[N:25]=[C:24]([NH:26][C:27](=[O:32])[C:28]([CH3:31])([CH3:30])[CH3:29])[C:23]([CH:33]=[O:34])=[CH:22][CH:21]=1.O>C1COCC1.C(OCC)(=O)C.[Cl-].[Na+].O>[C:15]([O:14][C:11](=[O:13])[CH2:12][CH:33]([C:23]1[C:24]([NH:26][C:27](=[O:32])[C:28]([CH3:30])([CH3:29])[CH3:31])=[N:25][C:20]([Cl:19])=[CH:21][CH:22]=1)[OH:34])([CH3:18])([CH3:17])[CH3:16]
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참가 물질

8

반응물 4

HCID 962WaterHCID 10908tert-Butyl acetateHCID 14708120N-(6-chloro-3-formylpyridin-2-yl)-2,2-dimethylpropanamideHCID 57426343Lithium bis(trimethylsilyl)amide

생성물 1

HCID 14708126Tert-butyl 3-[6-chloro-2-(2,2-dimethylpropanamido)pyridin-3-yl]-3-hydroxypropanoate수율 79%

시약·촉매·용매 3

HCID 8028
Tetrahydrofuran
용매
2회
HCID 8857Ethyl Acetate용매
HCID 57417360Sodium chloride; water용매

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온도
-78 °C

실험 절차

A first intermediate compound, 7-Chloro-1H-[1,8]naphthyridin-2-one, was produced as follows: To a stirred solution of lithium hexamethyldisilazane (26.3 mmol, 1.0 M in THF) in THF (10 mL) at −78° C. is added t-butyl acetate (3.53 mL, 26.3 mmol) dropwise. The mixture is stirred at −78° C. for 30 min and N-(6-chloro-3-formyl-pyridin-2-yl)-2,2-dimethyl-propionamide (3.00 g, 12.5 mmol) in THF (20 mL) is added dropwise. A yellow precipitate forms and the mixture is stirred at −78° C. for 30 minutes and warmed to room temperature over 3 hours. H2O (10 mL) is added, the mixture stirred for 5 minutes and then diluted with ethyl acetate (20 mL) and brine (10 mL). The organic layer is separated, washed with brine (20 mL), dried over Na2SO4, filtered and concentrated under vacuum. The compound is recrystallized from ethyl acetate and hexanes to yield 3-[6-chloro-2-(2,2-dimethyl-propionylamino)-pyridin-3-yl]-3-hydroxy-propionic acid tert-butyl ester (3.52 g, 79%); mp 130–132° C., 1H NMR (400 MHz, CDCl3) δ 8.25 (br s, 1H), 7.76 (d, 1H), 7.16 (d, 1H), 5.05–4.98 (m, 1H), 4.08 (d, 1H), 2.80 (dd, 1H), 2.70 (dd, 1H), 1.41 (s, 9H), 1.36 (s, 9H); MS ES+ 357.03 (M+H)+.

후처리

  1. stirringA yellow precipitate forms and the mixture is stirred at −78° C. for 30 minutes
  2. temperaturewarmed to room temperature over 3 hours
  3. stirringthe mixture stirred for 5 minutes
  4. customThe organic layer is separated
  5. washwashed with brine (20 mL)
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under vacuum
  9. customThe compound is recrystallized from ethyl acetate and hexanes

출처 및 근거

ORD 기록
ord-1a0a82ef850d45df845a756073b48948
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07160888B2

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