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Pivalic acid → 4-(5-(4-(Heptyloxy)phenyl)thiazol-2-yl)benzaldehyde

HRID 716404
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HRID 716404 반응식
[S:1]1[CH:5]=[CH:4][N:3]=[C:2]1[C:6]1[CH:13]=[CH:12][C:9]([CH:10]=[O:11])=[CH:8][CH:7]=1.C1(P(C2CCCCC2)C2CCCCC2)CCCCC1.C(O)(=O)C(C)(C)C.C(=O)([O-])[O-].[K+].[K+].Br[C:47]1[CH:52]=[CH:51][C:50]([O:53][CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH3:60])=[CH:49][CH:48]=1>CC(N(C)C)=O.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH2:54]([O:53][C:50]1[CH:49]=[CH:48][C:47]([C:5]2[S:1][C:2]([C:6]3[CH:7]=[CH:8][C:9]([CH:10]=[O:11])=[CH:12][CH:13]=3)=[N:3][CH:4]=2)=[CH:52][CH:51]=1)[CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH3:60]
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참가 물질

8

반응물 5

HCID 6417Pivalic acidHCID 11430Potassium CarbonateHCID 75806TricyclohexylphosphineHCID 5991021-(4-Bromophenoxy)heptaneHCID 105356554-(1,3-Thiazol-2-yl)benzaldehyde

생성물 1

HCID 866896684-(5-(4-(Heptyloxy)phenyl)thiazol-2-yl)benzaldehyde수율 38.7%

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 31374Dimethylacetamide용매2회

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온도
100 °C

실험 절차

To a stirring suspension of 4-(thiazol-2-yl)benzaldehyde (349 mg, 1.84 mmol), tricyclohexylphosphine (27 mg, 0.07 mmol), pivalic acid (64.2 μl, 0.55 mmol), potassium carbonate (382 mg, 2.77 mmol) and palladium (II) acetate (8 mg, 0.04 mmol) in DMA (5.15 mL) under nitrogen was added a solution of 1-bromo-4-(heptyloxy)benzene (500 mg, 1.84 mmol) in DMA (1 mL). The reaction mixture was evacuated and purged with nitrogen 3 times then heated at 100° C. for 6 h. Once cooled, the reaction mixture was diluted with EA (40 mL), washed with water (3×40 mL) and brine (40 mL). The organic phase was dried over MgSO4, filtered and concentrated in vacuo to afford a brown-green solid. The crude product was purified by chromatography (0-50% EA in hexanes) to afford 270 mg (37%) of 4-(5-(4-(heptyloxy)phenyl)thiazol-2-yl)benzaldehyde as an iridescent yellow solid. LCMS-ESI (m/z) calculated for C23H25NO2S: 379.5. found 380.0 [M+H]+, tR=2.99 min. (Method 8).

후처리

  1. customThe reaction mixture was evacuated
  2. custompurged with nitrogen 3 times
  3. temperatureOnce cooled
  4. additionthe reaction mixture was diluted with EA (40 mL)
  5. washwashed with water (3×40 mL) and brine (40 mL)
  6. dry with materialThe organic phase was dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customto afford a brown-green solid
  10. customThe crude product was purified by chromatography (0-50% EA in hexanes)

출처 및 근거

ORD 기록
ord-6314c09ef8654f6cb382e5359f1be58f
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09187522B2

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