2,4,6-Trimethylpyridine → HCID 56672028, 화합물

HRID 1914814노트

반응식

HRID 1914814 반응식
[C:1]([NH:5][C@H:6]1[CH2:10][CH2:9][C@@H:8]([C:11]([OH:13])=O)[CH2:7]1)(=[O:4])[CH2:2][CH3:3].ClC(N(C)C)=C(C)C.[CH3:22][NH:23][C:24]1[CH:29]=[CH:28][C:27]([C:30]2[N:34]([CH3:35])[C:33]3[CH:36]=[CH:37][CH:38]=[CH:39][C:32]=3[N:31]=2)=[CH:26][CH:25]=1.N1C(C)=CC(C)=CC=1C>C1COCC1.C(Cl)Cl>[CH3:22][N:23]([C:24]1[CH:29]=[CH:28][C:27]([C:30]2[N:34]([CH3:35])[C:33]3[CH:36]=[CH:37][CH:38]=[CH:39][C:32]=3[N:31]=2)=[CH:26][CH:25]=1)[C:11]([C@@H:8]1[CH2:9][CH2:10][C@H:6]([NH:5][C:1](=[O:4])[CH2:2][CH3:3])[CH2:7]1)=[O:13]

참가 물질

7

반응물 4

HCID 79532,4,6-TrimethylpyridineHCID 6407921-Chloro-N,N-2-trimethylpropenylamineHCID 13713019HCID 13713019, 화합물HCID 67112454HCID 67112454, 화합물

생성물 1

HCID 56672028HCID 56672028, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

100.0 mg (0.54 mmol) (1R,3S)-3-Propionylamino-cyclopentanecarboxylic acid (educt IV.1) and 78.6 μL (0.59 mmol) 1-chloro-N,N,2-trimethyl-propenylamine are stirred in 5 mL dry THF at RT for 1 hour. Then this mixture is given to a mixture of 128.1 mg (0.54 mmol) N-methyl-N-[4-(1-methyl-1H-benzoimidazol-2-yl)-phenyl]-amine (educt III.1.a) and 107.0 μL (0.81 mmol) 2,4,6-collidine in DCM at RT. The mixture is stirred over night. The solvent is evaporated. The residue is taken up with water and extracted with DCM. The organic phase is dried and the solvent is evaporated. The residue is triturated with diethyl ether, filtered off and dried.

후처리

  1. customThe solvent is evaporated
  2. extractionextracted with DCM
  3. customThe organic phase is dried
  4. customthe solvent is evaporated
  5. customThe residue is triturated with diethyl ether
  6. filtrationfiltered off
  7. customdried

출처 및 근거

ORD 기록
ord-78f86ecdc6dc4d908d0ac1b79d39b431
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08614238B2

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