Diisopropylethylamine → HCID 69013806、化合物

HRID 1371767ノート

反応式

HRID 1371767 の反応式
[NH2:1][CH:2]1[CH2:7][CH2:6][N:5]([S:8]([CH3:11])(=[O:10])=[O:9])[CH2:4][CH:3]1[OH:12].[NH2:13][C:14]1[C:19]([C:20]([C:22]2[C:27]([O:28][CH3:29])=[CH:26][CH:25]=[C:24]([F:30])[C:23]=2[F:31])=[O:21])=[CH:18][N:17]=[C:16](Cl)[N:15]=1.C(N(C(C)C)CC)(C)C>C(O)C>[NH2:13][C:14]1[C:19]([C:20]([C:22]2[C:27]([O:28][CH3:29])=[CH:26][CH:25]=[C:24]([F:30])[C:23]=2[F:31])=[O:21])=[CH:18][N:17]=[C:16]([NH:1][CH:2]2[CH2:7][CH2:6][N:5]([S:8]([CH3:11])(=[O:10])=[O:9])[CH2:4][CH:3]2[OH:12])[N:15]=1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 21070550HCID 21070550、化合物HCID 21070647HCID 21070647、化合物

生成物 1

HCID 69013806HCID 69013806、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The amine (44 mg, 0.22 mmol, Example 305) and chloropyrimidine (55 mg, 0.18 mmol, Example 289) were dissolved in ethanol (5 mL). To the stirred mixture at reflux, diisopropylethylamine (64 uL, Aldrich) was added and the mixture was refluxed for 20 hours. The solvent was removed and the residue was purified by HPLC (10–60%, acetonitrile/water) to give a white solid, 25 mg, 30%. MS (ES) MH+=458.

後処理

  1. temperatureTo the stirred mixture at reflux
  2. temperaturethe mixture was refluxed for 20 hours
  3. customThe solvent was removed
  4. customthe residue was purified by HPLC (10–60%, acetonitrile/water)
  5. customto give a white solid, 25 mg, 30%

出典と根拠

ORDレコード
ord-84151c360d744b4ebee4b462e0684f6c
出典データセット
uspto-grants-2007_01
特許番号
US07157455B2

反応ノート

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