1,3-Propanediamine, N1,N1,N3-trimethyl- → HCID 178483532、化合物

HRID 77099ノート

反応式

HRID 77099 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][CH:11]([C:14](O)=[O:15])[CH2:10][CH2:9]2)=[CH:4][C:3]=1[C:17]1[NH:21][C:20]2[CH:22]=[CH:23][C:24]([F:26])=[CH:25][C:19]=2[N:18]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH3:51][N:52]([CH3:58])[CH2:53][CH2:54][CH2:55][NH:56][CH3:57]>ClCCl>[CH3:51][N:52]([CH3:58])[CH2:53][CH2:54][CH2:55][N:56]([CH3:57])[C:14]([CH:11]1[CH2:10][CH2:9][N:8]([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[C:3]([C:17]3[NH:21][C:20]4[CH:22]=[CH:23][C:24]([F:26])=[CH:25][C:19]=4[N:18]=3)[CH:4]=2)[CH2:13][CH2:12]1)=[O:15]

参加物

5

反応物 3

HCID 783021,3-Propanediamine, N1,N1,N3-trimethyl-HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 1785245471-[4-Chloro-3-(5-fluoro-1H-benzoimidazol-2-yl)-phenyl]-piperidine-4-carboxylic acid

生成物 1

HCID 178483532HCID 178483532、化合物収率 49%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
35 °C

実験手順

Method H—Step a To a vial with 1-[4-Chloro-3-(5-fluoro-1H-benzoimidazol-2-yl)-phenyl]-piperidine-4-carboxylic acid (obtained as described in general method 3,4, step e) (0.10 g, 0.26 mmol) and HATU (0.10 g, 0.27 mmol) in dichloromethane (2 mL), TEA (0.07 mL, 0.54 mmol) and N,N,N′-trimethyl-1,3-propanediamine (0.32 mmol, 0.05 mL) were added. The reaction mixture was heated at 35° C. overnight, solvent was removed and the crude was purified by PrepHPLC and SCX column to obtain 0.06 g of the title compound (49%).

後処理

  1. customsolvent was removed
  2. customthe crude was purified by PrepHPLC and SCX column

出典と根拠

ORDレコード
ord-27ca3a58482c406992ccbeb17b6ca9cb
出典データセット
uspto-grants-2014_09
特許番号
US08835648B2

反応ノート

読み込み中…