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

Isopropyl iodide → Methyl 2-(2-(benzyloxy)-5-(1-isopropylpiperidin-4-yl)benzamido)-4-phenylbenzoate

HRID 454722
ノート
印刷プレビュー

反応式

HRID 454722 の反応式
[CH:1](I)([CH3:3])[CH3:2].[CH2:5]([O:12][C:13]1[CH:37]=[CH:36][C:35]([CH:38]2[CH2:43][CH2:42][NH:41][CH2:40][CH2:39]2)=[CH:34][C:14]=1[C:15]([NH:17][C:18]1[CH:27]=[C:26]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[CH:25]=[CH:24][C:19]=1[C:20]([O:22][CH3:23])=[O:21])=[O:16])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.C(=O)([O-])[O-].[K+].[K+]>C(=O)([O-])[O-].[K+].[K+].C(#N)C>[CH2:5]([O:12][C:13]1[CH:37]=[CH:36][C:35]([CH:38]2[CH2:39][CH2:40][N:41]([CH:1]([CH3:3])[CH3:2])[CH2:42][CH2:43]2)=[CH:34][C:14]=1[C:15]([NH:17][C:18]1[CH:27]=[C:26]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[CH:25]=[CH:24][C:19]=1[C:20]([O:22][CH3:23])=[O:21])=[O:16])[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6362Isopropyl iodide2 回HCID 11430Potassium CarbonateHCID 66990546Methyl 2-(2-(benzyloxy)-5-(piperidin-4-yl)benzamido)-4-phenylbenzoate

生成物 1

HCID 66989977Methyl 2-(2-(benzyloxy)-5-(1-isopropylpiperidin-4-yl)benzamido)-4-phenylbenzoate

試薬・触媒・溶媒 2

HCID 11430Potassium Carbonate触媒
HCID 6342
Acetonitrile
溶媒

実験手順

Potassium carbonate (0.033 mg) and isopropyl iodide (0.024 mL) were sequentially added to an acetonitrile (1.9 mL) suspension of methyl 2-(2-(benzyloxy)-5-(piperidin-4-yl)benzamido)-4-phenylbenzoate (0.13 g), followed by heating to reflux for 1 hour. The reaction mixture was cooled to room temperature, and potassium carbonate (6.7 mg) and isopropyl iodide (4.8 μL) were sequentially added thereto, followed by heating to reflux for 2 hours. After cooling the reaction mixture to room temperature, the solvent was evaporated under reduced pressure, and ethyl acetate and a saturated aqueous solution of sodium bicarbonate were added to the residue. The organic layer was separated, washed with a saturated aqueous solution of sodium chloride, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography [eluent: 100-95% chloroform/methanol] to obtain 0.12 g of methyl 2-(2-(benzyloxy)-5-(1-isopropylpiperidin-4-yl)benzamido)-4-phenylbenzoate as an orange oily sub stance.

後処理

  1. temperatureby heating
  2. temperatureto reflux for 1 hour
  3. temperatureby heating
  4. temperatureto reflux for 2 hours
  5. temperatureAfter cooling the reaction mixture to room temperature
  6. customthe solvent was evaporated under reduced pressure, and ethyl acetate
  7. additiona saturated aqueous solution of sodium bicarbonate were added to the residue
  8. customThe organic layer was separated
  9. washwashed with a saturated aqueous solution of sodium chloride
  10. dry with materialdried over anhydrous sodium sulfate
  11. customthe solvent was evaporated under reduced pressure
  12. customThe obtained residue was purified by silica gel column chromatography [eluent: 100-95% chloroform/methanol]

出典と根拠

ORDレコード
ord-b1dffccf4d49430e967614e7a35604ae
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08492582B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート