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Cesium carbonate → tert-butyl (5-methyl-1,3,4-thiadiazol-2-yl)methyl(2-methyl-6-(((1S,2S)-2-(5-methyl pyridin-2-yl)cyclopropyl)methoxy)-3-oxo-2,3-dihydropyridazin-4-yl)carbamate

HRID 530789
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HRID 530789 반응식
Br[C:2]1[C:3](=[O:21])[N:4]([CH3:20])[N:5]=[C:6]([O:8][CH2:9][C@H:10]2[CH2:12][C@@H:11]2[C:13]2[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][N:14]=2)[CH:7]=1.[CH3:22][C:23]1[S:27][C:26]([CH2:28][NH:29][C:30](=[O:36])[O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[N:25][N:24]=1.C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.C([O-])([O-])=O.[Cs+].[Cs+]>C1(C)C=CC=CC=1.CCOC(C)=O.CC([O-])=O.CC([O-])=O.[Pd+2]>[CH3:22][C:23]1[S:27][C:26]([CH2:28][N:29]([C:2]2[C:3](=[O:21])[N:4]([CH3:20])[N:5]=[C:6]([O:8][CH2:9][C@H:10]3[CH2:12][C@@H:11]3[C:13]3[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][N:14]=3)[CH:7]=2)[C:30](=[O:36])[O:31][C:32]([CH3:34])([CH3:33])[CH3:35])=[N:25][N:24]=1
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참가 물질

8

반응물 4

HCID 10796Cesium carbonateHCID 634876Binap, (A+-)-HCID 59892191Tert-butyl ((5-methyl-1,3,4-thiadiazol-2-yl)methyl)carbamateHCID 904543854-bromo-2-methyl-6-(((1S,2S)-2-(5-methylpyridin-2-yl)cyclopropyl)methoxy)pyridazin-3(2H)-one

생성물 1

HCID 131735649
tert-butyl (5-methyl-1,3,4-thiadiazol-2-yl)methyl(2-methyl-6-(((1S,2S)-2-(5-methyl pyridin-2-yl)cyclopropyl)methoxy)-3-oxo-2,3-dihydropyridazin-4-yl)carbamate

시약·촉매·용매 3

HCID 167845palladium(II) acetate촉매HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

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온도
85 °C

실험 절차

A mixture of 4-bromo-2-methyl-6-(((1S,2S)-2-(5-methylpyridin-2-yl)cyclopropyl)methoxy)pyridazin-3(2H)-one (5) (90 mg, 0.26 mmol), tert-butyl (5-methyl-1,3,4-thiadiazol-2-yl)methylcarbamate (6) (119 mg, 0.52 mmol), Pd(OAc)2 (9 mg, 0.052 mmol), BINAP (36 mg, 0.057 mmol) and Cs2CO3 (127 mg, 0.39 mmol) in toluene (4 mL) under N2 was heated at 85° C. for 20 h. After cooled to rt, The mixture was diluted with EtOAc (20 mL), washed with H2O and brine, dried over MgSO4, filtered and concentrated in vacuo. The residue was purified by column chromatography on silica gel, eluting with PE/EA (1/2) to give the title compound as a oil.

후처리

  1. temperatureAfter cooled to rt
  2. washwashed with H2O and brine
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by column chromatography on silica gel
  7. washeluting with PE/EA (1/2)

출처 및 근거

ORD 기록
ord-f5042f8e75db4d319361620cf8a02e65
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09353104B2

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