Triphenylphosphine → HCID 68294314, 화합물

HRID 1850075노트

반응식

HRID 1850075 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[NH:20]1[CH:24]=[C:23](/[CH:25]=[CH:26]/[C:27]([O:29][CH3:30])=[O:28])[CH:22]=[N:21]1.[CH3:31][N:32]1[CH2:37][CH2:36][CH:35]([CH2:38]O)[CH2:34][CH2:33]1.N(C(OC(C)(C)C)=O)=NC(OC(C)(C)C)=O>O1CCCC1>[CH3:31][N:32]1[CH2:37][CH2:36][CH:35]([CH2:38][N:20]2[CH:24]=[C:23](/[CH:25]=[CH:26]/[C:27]([O:29][CH3:30])=[O:28])[CH:22]=[N:21]2)[CH2:34][CH2:33]1

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 97268Di-tert-butyl azodicarboxylateHCID 2719711-Methyl-4-piperidinemethanolHCID 68295278HCID 68295278, 화합물

생성물 1

HCID 68294314HCID 68294314, 화합물수율 84%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Triphenylphosphine (393 mg, 1.5 mmol) and (E)-methyl 3-(1H-pyrazol-4-yl)acrylate, prepared as described above, (12 mg, 1 mmol) were added to a solution of N-methyl-4-hydroxymethyl-piperidine (165 mg, 1.25 mmol) in tetrahydrofuran (THF, 2 mL). After addition of di-tert-butyl azodicarboxylate (345 mg, 1.5 mmol), the reaction was stirred overnight at room temperature. Solvents were evaporated under reduced pressure and the residue was purified by silica gel chromatography using a gradient of Hexane in EtOAc from 1:1 to 0:100 v/v. Fractions containing product were pooled and evaporated to give 220 mg of pure material (0.84 mmol, 84%).

후처리

  1. customSolvents were evaporated under reduced pressure
  2. customthe residue was purified by silica gel chromatography
  3. additionFractions containing product
  4. customevaporated

출처 및 근거

ORD 기록
ord-eb1833eaac4b4f5d9df9114d5309d980
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957066B2

반응 노트

불러오는 중…