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tert-Butyl piperazine-1-carboxylate → Tert-butyl 4-(4-(pyrrolidin-1-yl)quinazolin-7-yl)piperazine-1-carboxylate

HRID 2090812
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HRID 2090812 반응식
CC(C)([O-])C.[K+].C1(P(C2CCCCC2)C2(C(C)C)CC(C(C)C)=CC(C(C)C)=C2C2C=CC=CC=2)CCCCC1.Cl[C:42]1[CH:51]=[C:50]2[C:45]([C:46]([N:52]3[CH2:56][CH2:55][CH2:54][CH2:53]3)=[N:47][CH:48]=[N:49]2)=[CH:44][CH:43]=1.[N:57]1([C:63]([O:65][C:66]([CH3:69])([CH3:68])[CH3:67])=[O:64])[CH2:62][CH2:61][NH:60][CH2:59][CH2:58]1>C1(C)C=CC=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.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C(OCC)(=O)C.O>[N:52]1([C:46]2[C:45]3[C:50](=[CH:51][C:42]([N:60]4[CH2:59][CH2:58][N:57]([C:63]([O:65][C:66]([CH3:69])([CH3:68])[CH3:67])=[O:64])[CH2:62][CH2:61]4)=[CH:43][CH:44]=3)[N:49]=[CH:48][N:47]=2)[CH2:56][CH2:55][CH2:54][CH2:53]1
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참가 물질

9

반응물 4

HCID 143452tert-Butyl piperazine-1-carboxylateHCID 17479737HCID 17479737, 화합물HCID 23665647Potassium tert-butoxideHCID 672859322-Dicyclohexylphosphino-2,4,6-triisopropylbiphenyl

생성물 1

HCID 59746514Tert-butyl 4-(4-(pyrrolidin-1-yl)quinazolin-7-yl)piperazine-1-carboxylate

시약·촉매·용매 4

HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 962Water용매
HCID 1140Toluene용매
HCID 8857Ethyl Acetate용매

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온도
100 °C

실험 절차

Potassium tert-butoxide (998 mg, 8.99 mmol), 2-dicyclohexylphosphino-2,4,6-triisopropyl-biphenyl (X-Phos) (79 mg, 0.18 mmol) and tris-(dibenzylideneacetone)-dipalladium [Pd2(dba)3] (36 mg, 0.036 mmol) were added, under nitrogen, to a mixture of 7-chloro-4-(pyrrolidin-1-yl)quinazoline (A) (840 mg, 3.59 mmol) and tert-butyl piperazine-1-carboxylate (1.0 g, 5.39 mmol) in toluene (49 ml). The reaction mixture was then heated for 15 h at 100° C. The reaction mixture was cooled to room temperature, and water (25 ml) and ethyl acetate (25 ml) were added. The aqueous phase was extracted with ethyl acetate (2×25 ml), and the combined organic phases were washed with saturated sodium chloride solution (20 ml). The organic phase was then dried (MgSO4) and concentrated in vacuo. The crude product was purified by column chromatography (silica gel) using ethyl acetate/-dichloromethane/ammonia solution (25% aq.) (50:10:0.5) and ethyl acetate/dichloro-methane/methyl tert-butyl ether/ammonia solution (25% aq.) (50:10:10:0.7).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionThe aqueous phase was extracted with ethyl acetate (2×25 ml)
  3. washthe combined organic phases were washed with saturated sodium chloride solution (20 ml)
  4. dry with materialThe organic phase was then dried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customThe crude product was purified by column chromatography (silica gel)

출처 및 근거

ORD 기록
ord-21ec4c1f22c14a65a569bc67b5d27e3f
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08435978B2

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