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

HRID 1255302ノート

反応式

HRID 1255302 の反応式
C(P1(=O)OP(CCC)(=O)OP(CCC)(=O)[O:5]1)CC.[CH:19]([C:22]1[S:23][CH:24]=[C:25]([C:27]([N:29]2[CH2:34][C:33]3([CH2:39][CH2:38][N:37]([CH2:40][CH2:41][C:42]4[CH:55]=[CH:54][C:45]([CH2:46][CH2:47][O:48][CH2:49]CC(O)=O)=[CH:44][CH:43]=4)[CH2:36][CH2:35]3)[O:32][CH2:31][CH2:30]2)=[O:28])[N:26]=1)([CH3:21])[CH3:20].[CH2:56]([NH:58][CH2:59][CH:60]([O:63][CH3:64])[O:61][CH3:62])[CH3:57].C(N([CH2:70][CH3:71])CC)C>CN(C=O)C>[CH3:62][O:61][CH:60]([O:63][CH3:64])[CH2:59][N:58]([CH2:70][CH3:71])[C:56](=[O:5])[CH2:57][CH2:49][O:48][CH2:47][CH2:46][C:45]1[CH:54]=[CH:55][C:42]([CH2:41][CH2:40][N:37]2[CH2:38][CH2:39][C:33]3([O:32][CH2:31][CH2:30][N:29]([C:27]([C:25]4[N:26]=[C:22]([CH:19]([CH3:21])[CH3:20])[S:23][CH:24]=4)=[O:28])[CH2:34]3)[CH2:35][CH2:36]2)=[CH:43][CH:44]=1

参加物

6

反応条件

温度
20 °C

実験手順

T3P (1.6M in THF, 0.33 mL) was added dropwise to a stirred 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-ethyl-2,2-dimethoxyethanamine [U.S. Pat. No. 2,707,186] (0.062 g) and triethylamine (0.46 mL) in DMF (7 mL). The reaction mixture was stirred at 20° C. for 3 hours. The mixture was partitioned between ethyl acetate and brine, the organic layer was washed with brine (×2), dried, filtered and the solvent evaporated under reduced pressure to yield the subtitled compound.

後処理

  1. customThe mixture was 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-84ea1f1490054ccd95a30450adeebc68
出典データセット
uspto-grants-2013_06
特許番号
US08455483B2

反応ノート

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