Diisopropylethylamine → HCID 67304739, 화합물

HRID 535034노트

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HRID 535034 반응식
[C:1]([O:5][C:6]([CH:8]1[CH2:13][CH2:12][CH2:11][NH:10][CH:9]1[C:14]([OH:16])=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH:17]([C:20]1[CH:21]=[C:22]([C:26]2[CH2:27][CH2:28][NH:29][CH2:30][CH:31]=2)[CH:23]=[CH:24][CH:25]=1)([CH3:19])[CH3:18].C1CN([P+](ON2N=NC3C=CC=CC2=3)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F.C(N(C(C)C)CC)(C)C>CN(C=O)C.CCOC(C)=O>[C:1]([O:5][C:6]([CH:8]1[CH2:13][CH2:12][CH2:11][NH:10][CH:9]1[C:14]([N:29]1[CH2:28][CH:27]=[C:26]([C:22]2[CH:23]=[CH:24][CH:25]=[C:20]([CH:17]([CH3:19])[CH3:18])[CH:21]=2)[CH2:31][CH2:30]1)=[O:16])=[O:7])([CH3:2])([CH3:3])[CH3:4]

참가 물질

7

반응물 4

HCID 81531DiisopropylethylamineHCID 2724699PyBOPHCID 22956954HCID 22956954, 화합물HCID 673051604-(3-Isopropyl-phenyl)-1,2,3,6-tetrahydro-pyridine

생성물 1

HCID 67304739HCID 67304739, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a 0° C. solution of piperidine-2,3-dicarboxylic acid 3-tert-butyl ester (100 mg) in DMF (0.6 mL) was added sequentially, 4-(3-isopropyl-phenyl)-1,2,3,6-tetrahydro-pyridine (97 mg), PyBOP (232 mg), and diisopropylethylamine (0.152 mL). The resultant mixture was stirred at rt overnight. The reaction solution was diluted with EtOAc and washed with saturated NaHCO3 solution (×3), water, and brine. The organic layers were dried over MgSO4, filtered, and concentrated to dry under reduced pressure. The residue was used in next step without further purifications. MS (ESI): 413.2 (M+H+)

후처리

  1. washwashed with saturated NaHCO3 solution (×3), water, and brine
  2. dry with materialThe organic layers were dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customto dry under reduced pressure

출처 및 근거

ORD 기록
ord-25686d4621a245fc8f83700781d74909
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08853243B2

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