ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Sodium Carbonate → methyl 2-[3-(acetylamino)-2-aminophenyl]-3-cyclohexyl-1H-indole-6-carboxylate

HRID 1518229
ノート
印刷プレビュー

反応式

HRID 1518229 の反応式
[C:1]([NH:4][C:5]1[C:6]([NH2:14])=[C:7](B(O)O)[CH:8]=[CH:9][CH:10]=1)(=[O:3])[CH3:2].Br[C:16]1[NH:17][C:18]2[C:23]([C:24]=1[CH:25]1[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]1)=[CH:22][CH:21]=[C:20]([C:31]([O-:33])=[O:32])[CH:19]=2.N1C2C(=CC=C(C(OC)=O)C=2)C=[CH:35]1.C([O-])([O-])=O.[Na+].[Na+]>O1CCOCC1.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[C:1]([NH:4][C:5]1[C:6]([NH2:14])=[C:7]([C:16]2[NH:17][C:18]3[C:23]([C:24]=2[CH:25]2[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]2)=[CH:22][CH:21]=[C:20]([C:31]([O:33][CH3:35])=[O:32])[CH:19]=3)[CH:8]=[CH:9][CH:10]=1)(=[O:3])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 10340Sodium CarbonateHCID 639844Methyl indole-6-carboxylateHCID 53692531[3-(Acetylamino)-2-aminophenyl]boronic acidHCID 863099302-bromo-3-cyclohexyl-1H-indole-6-carboxylate

生成物 1

HCID 68708755methyl 2-[3-(acetylamino)-2-aminophenyl]-3-cyclohexyl-1H-indole-6-carboxylate収率 59%

試薬・触媒・溶媒 2

HCID 178418476HCID 178418476、化合物触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
105 °C

実験手順

[3-(acetylamino)-2-aminophenyl]boronic acid (prepared as described in Example 5, Step 1 above) (1.1 eq) was added to a solution of 2-bromo-3-cyclohexyl-1H-indole-6-carboxylate (prepared from commercially available methyl indole-6-carboxylate as described in WO 2004/087714) in dioxane (0.06 M). 2M aqueous Na2CO3 (4 eq) was introduced and the mixture degassed by sonication under a N2 atmosphere prior to introducing bis(triphenylphosphine)palladium(II) dichloride (0.2 eq) and heating at 105° C. for 2 h. The reaction was allowed to cool to RT before partitioning between EtOAc and water. The aqueous phase was extracted a second time with EtOAc and the combined organics washed with water, brine before being dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. Purification by flash chromatography (5% MeOH/CH2Cl2) afforded the title compound as a glass (59%). MS (ES+) m/z 406 (M+H)+.

後処理

  1. customthe mixture degassed by sonication under a N2 atmosphere
  2. temperatureto cool to RT
  3. custombefore partitioning between EtOAc and water
  4. extractionThe aqueous phase was extracted a second time with EtOAc
  5. washthe combined organics washed with water, brine
  6. dry with materialbefore being dried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customPurification by flash chromatography (5% MeOH/CH2Cl2)

出典と根拠

ORDレコード
ord-e6d1dbf9dbfb4baa9fc1559daab62ff8
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08232390B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート