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Ammonium Chloride → 5-[4-(1-hydroxycyclobutyl)phenyl]-6-methyl-1H-indole-3-carbaldehyde

HRID 1054657
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HRID 1054657 반응식
[CH:1]1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC)=CC=CC=2OC)CCCCC1.O.P([O-])([O-])([O-])=O.[K+].[K+].[K+].CB(O)O.Cl[C:44]1[CH:52]=[C:51]2[C:47]([C:48]([CH:53]=[O:54])=[CH:49][NH:50]2)=[CH:46][C:45]=1[C:55]1[CH:60]=[CH:59][C:58]([C:61]2([OH:65])[CH2:64][CH2:63][CH2:62]2)=[CH:57][CH:56]=1.[Cl-].[NH4+]>O1CCOCC1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[OH:65][C:61]1([C:58]2[CH:57]=[CH:56][C:55]([C:45]3[CH:46]=[C:47]4[C:51](=[CH:52][C:44]=3[CH3:1])[NH:50][CH:49]=[C:48]4[CH:53]=[O:54])=[CH:60][CH:59]=2)[CH2:64][CH2:63][CH2:62]1
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참가 물질

8

반응물 5

HCID 25517Ammonium ChlorideHCID 139377Methylboronic AcidHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenylHCID 22031701Potassium phosphate, tribasic, monohydrateHCID 866985686-Chloro-5-(4-(1-hydroxycyclobutyl)phenyl)-1H-indole-3-carbaldehyde

생성물 1

HCID 86698661
5-[4-(1-hydroxycyclobutyl)phenyl]-6-methyl-1H-indole-3-carbaldehyde

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 312751,4-Dioxane용매

실험 절차

A mixture of dicyclohexyl(2′,6′-dimethoxybiphenyl-2-yl)phosphane (62.8 mg, 0.153 mmol), palladium acetate (13.7 mg, 0.061 mmol), tribasic potassium phosphate monohydrate (566 mg, 2.46 mmol), and methyl boronic acid (184 mg, 3.07 mmol) was sealed in a microwave tube and evacuated and backfilled with nitrogen three times. Deoxygenated 1,4-dioxane (1.5 mL) was added and the mixture was stirred vigorously at room temperature for one hour. A solution of 6-chloro-5-[4-(1-hydroxy-cyclobutyl)-phenyl]-1H-indole-3-carbaldehyde (400 mg, 1.23 mmol) in 1,4-dioxane (2.5 mL) was degassed with nitrogen for 10 minutes then added to the reaction mixture. The reaction mixture was heated at 120° C. for three hours under microwave irradiation, and then allowed to stir at room temperature for 12 hours. The reaction mixture was poured into saturated ammonium chloride solution (20 mL) and extracted with ethyl acetate (3×20 mL). The combined organic layers were dried over sodium sulfate, filtered and evaporated. Flash silica gel chromatography was performed on the crude product utilizing a solvent system of heptanes/ethyl acetate (9:1 to 1:1) to give the title compound. MS (ES+) 306.5 (M+H)+. 1H NMR (400 MHz, CD3OD) δ 9.86 (s, 1H), 8.06 (s, 1H), 7.95 (s, 1H), 7.55 (d, 2H), 7.38 (s, 1H), 7.36 (d, 2H), 2.61 (m, 2H), 2.39 (m, 2H), 2.34 (s, 3H), 2.05 (m, 1H), 1.75 (m, 1H).

후처리

  1. customwas sealed in a microwave tube
  2. customevacuated
  3. additionDeoxygenated 1,4-dioxane (1.5 mL) was added
  4. additionthen added to the reaction mixture
  5. temperatureThe reaction mixture was heated at 120° C. for three hours under microwave irradiation
  6. stirringto stir at room temperature for 12 hours
  7. extractionextracted with ethyl acetate (3×20 mL)
  8. dry with materialThe combined organic layers were dried over sodium sulfate
  9. filtrationfiltered
  10. customevaporated

출처 및 근거

ORD 기록
ord-320b2def7e6b4eb8a8c7614e6bf179b3
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09394285B2

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