Hydrochloric Acid → HCID 66751287, 화합물

HRID 535025

반응식

HRID 535025 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([C:8]([N:10]2[CH2:15][CH2:14][N:13]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[C:22]([CH3:25])([CH3:24])[CH3:23])[CH2:12][CH2:11]2)=[O:9])=[CH:4][CH:3]=1.CC1(C)C(C)(C)OB([C:34]2[CH:39]=[CH:38][C:37]([CH2:40][C:41]([OH:43])=[O:42])=[CH:36][CH:35]=2)O1.C(=O)([O-])[O-].[Na+].[Na+].Cl>O1CCCC1.C1(C)C=CC=CC=1.C(O)C.C(OCC)(=O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:22]([C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=1[N:13]1[CH2:14][CH2:15][N:10]([C:8]([C:5]2[CH:6]=[CH:7][C:2]([C:34]3[CH:39]=[CH:38][C:37]([CH2:40][C:41]([OH:43])=[O:42])=[CH:36][CH:35]=3)=[CH:3][CH:4]=2)=[O:9])[CH2:11][CH2:12]1)([CH3:25])([CH3:24])[CH3:23]

참가 물질

9

반응물 4

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 37190022-(4-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)acetic AcidHCID 66750884HCID 66750884, 화합물

생성물 1

HCID 66751287HCID 66751287, 화합물수율 26.4%

시약·촉매·용매 4

HCID 178418397HCID 178418397, 화합물촉매HCID 1140Toluene용매HCID 8028Tetrahydrofuran용매HCID 21584252Ethanol ethylacetate용매

반응 조건

온도
120 °C

실험 절차

A mixture of 1-[(4-bromophenyl)carbonyl]-4-(2-tert-butylphenyl)piperazine (1.0 g, 2.49 mmol), [4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]acetic acid (0.653 g, 2.49 mmol), 2 M sodium carbonate solution (3 mL, 6.0 mmol), and tetrakis(triphenylphosphine)palladium(0) (0.150 g, 0.13 mmol) in tetrahydrofuran (5 mL) and toluene (20 mL) was stirred at 120° C. for 16 h. 6 M hydrochloric acid solution was added and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to afford a solid. The solid was dissolved in ethanol-ethyl acetate and recrystallized to obtain a solid (0.3 g, 26%).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customto afford a solid
  7. customrecrystallized

출처 및 근거

ORD 기록
ord-728f5dec0c8547e88c4584c694190c2e
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08853215B2

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