Triethylamine → N-cyclohexyl-N-(2,2-dimethoxyethyl)-3-(4-(2-(4-(2-isopropylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)ethyl)phenethoxy)propanamide

HRID 446425ノート

反応式

HRID 446425 の反応式
CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH:25]([C:28]1[S:29][CH:30]=[C:31]([C:33]([N:35]2[CH2:40][C:39]3([CH2:45][CH2:44][N:43]([CH2:46][CH2:47][C:48]4[CH:61]=[CH:60][C:51]([CH2:52][CH2:53][O:54][CH2:55][CH2:56][C:57](O)=[O:58])=[CH:50][CH:49]=4)[CH2:42][CH2:41]3)[O:38][CH2:37][CH2:36]2)=[O:34])[N:32]=1)([CH3:27])[CH3:26].[CH3:62][O:63][CH:64]([O:73][CH3:74])[CH2:65][NH:66][CH:67]1[CH2:72][CH2:71][CH2:70][CH2:69][CH2:68]1.C(N(CC)CC)C>CN(C=O)C>[CH:67]1([N:66]([CH2:65][CH:64]([O:73][CH3:74])[O:63][CH3:62])[C:57](=[O:58])[CH2:56][CH2:55][O:54][CH2:53][CH2:52][C:51]2[CH:60]=[CH:61][C:48]([CH2:47][CH2:46][N:43]3[CH2:42][CH2:41][C:39]4([O:38][CH2:37][CH2:36][N:35]([C:33]([C:31]5[N:32]=[C:28]([CH:25]([CH3:26])[CH3:27])[S:29][CH:30]=5)=[O:34])[CH2:40]4)[CH2:45][CH2:44]3)=[CH:49][CH:50]=2)[CH2:72][CH2:71][CH2:70][CH2:69][CH2:68]1

参加物

6

反応条件

温度
20 °C

実験手順

HATU (0.23 g) was added in one portion to an ice cold solution of 3-(4-(2-(4-(2-isopropylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)ethyl)phenethoxy)propanoic acid [Example 1, step e] (0.3 g) and N-(2,2-dimethoxyethyl)cyclohexanamine [WO 2008075025] (0.087 g) and triethylamine (0.26 mL) in DMF (10 mL). The mixture was stirred at 20° C. for 1 hour before being partitioned between ethyl acetate and brine. The organic layer was washed with brine (×2), dried, filtered and the solvent evaporated under reduced pressure to afford the subtitled compound. Yield 0.32 g.

後処理

  1. custombefore being partitioned between ethyl acetate and brine
  2. washThe organic layer was washed with brine (×2)
  3. customdried
  4. filtrationfiltered
  5. customthe solvent evaporated under reduced pressure

出典と根拠

ORDレコード
ord-df97e2dd95814a03acfe0e6acac4156e
出典データセット
uspto-grants-2013_07
特許番号
US08476265B2

反応ノート

読み込み中…