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Isobutyronitrile → HCID 178448868, 화합물

HRID 707310
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HRID 707310 반응식
C(NC(C)C)(C)C.C([Li])CCC.[C:13](#[N:17])[CH:14]([CH3:16])[CH3:15].[S:18]1[C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=2[N:20]=[C:19]1[NH:27][C@H:28]1[CH2:31][C@H:30]([NH:32][C:33]2[C:38](Cl)=[N:37][CH:36]=[CH:35][N:34]=2)[CH2:29]1>CC(P(C(C)(C)C)C(C)(C)C)(C)C.CC(P(Br)(Br)(C(C)(C)C)C(C)(C)C)(C)C.[Pd].[Pd]>[S:18]1[C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=2[N:20]=[C:19]1[NH:27][C@H:28]1[CH2:31][C@H:30]([NH:32][C:33]2[C:38]([C:14]([CH3:16])([CH3:15])[C:13]#[N:17])=[N:37][CH:36]=[CH:35][N:34]=2)[CH2:29]1
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참가 물질

6

반응물 4

HCID 6559IsobutyronitrileHCID 7912DiisopropylamineHCID 178418339ButyllithiumHCID 178478364HCID 178478364, 화합물2회

생성물 1

HCID 178448868HCID 178448868, 화합물수율 40.7%

시약·촉매·용매 1

HCID 91885345
Dibromobis(tri-tert-butylphosphine)dipalladium(I)
촉매

실험 절차

Dibromobis(tri-tert-butylphosphine)dipalladium(I) (0.031 g, 0.040 mmol) was sealed in a microwave vessel under argon. Diisopropylamine (0.200 ml, 1.427 mmol) was added and the mixture cooled in a dry ice bath. A nitrogen needle was added followed by dropwise addition of butyllithium solution (2.5 m in hexanes, 0.500 ml, 1.250 mmol). The mixture was stirred for 5 minutes then isobutyronitrile (0.100 ml, 1.114 mmol) was added. The reaction was removed from the cold bath and allowed to slowly warm to room temperature. A solution of trans-N1-(benzo[d]thiazol-2-yl)-N3-(3-chloropyrazin-2-yl)cyclobutane-1,3-diamine (intermediate 27, 0.150 g, 0.452 mmol) in dry, sparged dioxane (1.5 mL) was added and the nitrogen needle removed. The reaction was heated at 95° C. for 14 hours. The crude was partitioned between water (100 mL), saturated ammonium chloride (10 mL) and ethyl acetate (200 mL). The organic phase was dried with magnesium sulfate and evaporated to dryness under reduced pressure. Purification using silica chromatography (dichloromethane to ethyl acetate gradient) gave the desired 2-(3-((trans-3-(benzo[d]thiazol-2-ylamino)cyclobutyl)amino)pyrazin-2-yl)-2-methylpropanenitrile (0.067 g, 0.184 mmol, 40.7% yield).

후처리

  1. temperaturethe mixture cooled in a dry ice bath
  2. additionA nitrogen needle was added
  3. customThe reaction was removed from the cold bath
  4. customsparged dioxane (1.5 mL)
  5. additionwas added
  6. customthe nitrogen needle removed
  7. temperatureThe reaction was heated at 95° C. for 14 hours
  8. customThe crude was partitioned between water (100 mL), saturated ammonium chloride (10 mL) and ethyl acetate (200 mL)
  9. dry with materialThe organic phase was dried with magnesium sulfate
  10. customevaporated to dryness under reduced pressure
  11. customPurification

출처 및 근거

ORD 기록
ord-75934e0d8d3a4a10b12debcda5af836b
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09174992B2

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