Diisopropylethylamine → HCID 131737175、化合物

HRID 61425ノート

反応式

HRID 61425 の反応式
[C:1]([O:5][C:6]([CH:8]1[CH2:13][CH2:12][CH2:11][NH:10][CH:9]1C(O)=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]NCC=2)[CH:23]=[CH:24][CH:25]=1)([CH3:19])[CH3:18].C1CN([P+]([O:48]N2N=NC3C=CC=CC2=3)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F.[CH:65]([N:68]([CH:71](C)C)CC)(C)[CH3:66]>CN(C=O)C.CCOC(C)=O>[C:1]([O:5][C:6]([CH:8]1[CH:13]([C:71]([N:68]2[CH2:65][CH:66]=[CH:28][CH2:27][CH:26]2[C:22]2[CH:23]=[CH:24][CH:25]=[C:20]([CH:17]([CH3:18])[CH3:19])[CH:21]=2)=[O:48])[CH2:12][CH2:11][NH:10][CH2:9]1)=[O:7])([CH3:2])([CH3:3])[CH3:4]

参加物

7

反応物 4

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

生成物 1

HCID 131737175HCID 131737175、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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-tetrahydropyridine (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+)

後処理

  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

出典と根拠

ORDレコード
ord-b9786a318b304490bf004bef6f1818a3
出典データセット
uspto-grants-2016_09
特許番号
US09440958B2

反応ノート

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