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1,2-Dimethoxyethane → Methyl 3-(2-hydroxypropan-2-yl)-1-(thiophen-3-yl)-1H-indazole-6-carboxylate

HRID 1047638
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HRID 1047638 반응식
[CH2:1]=[C:2]([C:4]1[C:12]2[C:7](=[CH:8][C:9]([C:13]([O:15][CH3:16])=[O:14])=[CH:10][CH:11]=2)[N:6]([C:17]2[CH:21]=[CH:20][S:19][CH:18]=2)[N:5]=1)[CH3:3].[BH4-].C([N+](CC)(CC)CC)C.C(COC)[O:33]C>CO.C1C=CC(C2C3=NC(C=C3)=C(C3C=CC=CC=3)C3[N-]C(=CC=3)C(C3C=CC=CC=3)=C3C=CC(=N3)C(C3C=CC=CC=3)=C3[N-]C=2C=C3)=CC=1.[Co+2]>[OH:33][C:2]([C:4]1[C:12]2[C:7](=[CH:8][C:9]([C:13]([O:15][CH3:16])=[O:14])=[CH:10][CH:11]=2)[N:6]([C:17]2[CH:21]=[CH:20][S:19][CH:18]=2)[N:5]=1)([CH3:3])[CH3:1]
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참가 물질

6

반응물 3

HCID 80711,2-DimethoxyethaneHCID 28251Tetraethylammonium tetrahydroborateHCID 66661623Methyl 3-(prop-1-en-2-yl)-1-(thiophen-3-yl)-1H-indazole-6-carboxylate

생성물 1

HCID 66661520Methyl 3-(2-hydroxypropan-2-yl)-1-(thiophen-3-yl)-1H-indazole-6-carboxylate수율 80%

시약·촉매·용매 2

HCID 518893
meso-Tetraphenylporphine-Co(II)
촉매
HCID 887Methanol용매

실험 절차

Methyl 3-(prop-1-en-2-yl)-1-(thiophen-3-yl)-1H-indazole-6-carboxylate (1.0763 g, 3.61 mmol) was dissolved in dimethoxyethane (90 ml)/MeOH (90 ml) at 25° C. Cobalt(II) meso-tetraphenylporphine (25.6 mg, 0.038 mmol) and tetraethylammonium borohydride (1.316 g, 9.07 mmol) were added sequentially. The reaction mixture was allowed to stir for 1.25 h. The reaction was stopped, quenched by addition of saturated aqueous ammonium chloride (100 mL), and the mixture extracted with ethyl acetate (3×80 mL). The combined organic phases were washed with saturated aqueous sodium chloride (1×80 mL), dried (sodium sulfate), filtered, and the solvent evaporated under reduced pressure. The crude product was purified by flash chromatography (RediSep SiO2, 330 g column) on a CombiFlash Rf purification system eluting with ethyl acetate-hexanes (0-45%). The title compound (912.2 mg, 2.88 mmol, 80% yield) was recovered as an orange solid. LC-MS: [M+1]=317.1.

후처리

  1. customquenched by addition of saturated aqueous ammonium chloride (100 mL)
  2. extractionthe mixture extracted with ethyl acetate (3×80 mL)
  3. washThe combined organic phases were washed with saturated aqueous sodium chloride (1×80 mL)
  4. dry with materialdried (sodium sulfate)
  5. filtrationfiltered
  6. customthe solvent evaporated under reduced pressure
  7. customThe crude product was purified by flash chromatography (RediSep SiO2, 330 g column) on a CombiFlash Rf purification system
  8. washeluting with ethyl acetate-hexanes (0-45%)

출처 및 근거

ORD 기록
ord-18cb3265a838422c81948ecfad00141c
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08569512B2

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