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4-Chloroaniline → 1-(4-Chlorophenylamino)-4-(4-pyridylmethoxy)pyridazine

HRID 1070536
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HRID 1070536 반응식
Br[N:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:9][C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)=[CH:4][NH:3]1.[Cl:16][C:17]1[CH:23]=[CH:22][C:20]([NH2:21])=[CH:19][CH:18]=1.C(OC(C)(C)C)(C)(C)C.[Na]>C1(C)C=CC=CC=1.C(OCC)(=O)C.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[Cl:16][C:17]1[CH:23]=[CH:22][C:20]([NH:21][N:2]2[CH:7]=[CH:6][C:5]([O:8][CH2:9][C:10]3[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=3)=[CH:4][NH:3]2)=[CH:19][CH:18]=1
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참가 물질

7

반응물 3

HCID 78124-ChloroanilineHCID 223972771-Bromo-4-(4-pyridylmethoxy)pyridazineHCID 86662868Sodium t-butyloxide

생성물 1

HCID 223972801-(4-Chlorophenylamino)-4-(4-pyridylmethoxy)pyridazine수율 10%

시약·촉매·용매 3

HCID 9811564Bis(dibenzylideneacetone)palladium촉매
HCID 1140
Toluene
용매
HCID 8857Ethyl Acetate용매

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온도
80 °C

실험 절차

To 1-bromo-4-(4-pyridylmethoxy)pyridazine (50 mg, 0.19 mmol) in toluene (3 mL) was added 4-chloroaniline (29 mg, 0.22 mmol), catalytical amount of (R)-(+)2,2′-bis(diphenyl phosphino)-1,1′-binaphthyl (1 mg), tris(dibenzylideneacetone)-dipalladium(0) (0.6 mg) and sodium t-butyloxide (26 mg, 0.27 mmol). The reaction mixture was heated at 80° C. for 12 h under argon. The reaction mixture became deep brown upon heating. The mixture was cooled to RT, diluted with ethyl acetate (10 mL), washed by brine and the organic layer was dried over Na2SO4, and the solvent was evaporated in vacuo. The crude mixture was purified by preparative thin layer plate to afford the title compound (6 mg, yield 10%). 1H-NMR (MeOH-4), 8.51 (d, 2H), 7.61(d, 2H) 7.52(dd, 2H), 7.15-7.25(m, 4H), 5.49(s, 2H); MS ES 313 (M+H)+, 315 (M+3H)+, 316 (M+4H)+, calc. 312; TLC (5:95 v/v methanol-methylene chloride) Rf=0.2.

후처리

  1. temperatureupon heating
  2. temperatureThe mixture was cooled to RT
  3. washwashed by brine
  4. dry with materialthe organic layer was dried over Na2SO4
  5. customthe solvent was evaporated in vacuo
  6. customThe crude mixture was purified by preparative thin layer plate

출처 및 근거

ORD 기록
ord-ce55ff32496e413aa622f1323061cad3
출처 데이터셋
uspto-grants-2005_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06903101B1

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