2,4,6-Trimethylpyridine → HCID 56672028、化合物

HRID 1914814ノート

反応式

HRID 1914814 の反応式
[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]

参加物

7

反応物 4

HCID 79532,4,6-TrimethylpyridineHCID 6407921-Chloro-N,N-2-trimethylpropenylamineHCID 13713019HCID 13713019、化合物HCID 67112454HCID 67112454、化合物

生成物 1

HCID 56672028HCID 56672028、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-78f86ecdc6dc4d908d0ac1b79d39b431
出典データセット
uspto-grants-2013_12
特許番号
US08614238B2

反応ノート

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