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Potassium Iodide → HCID 57253530、化合物

HRID 584241
ノート
印刷プレビュー

反応式

HRID 584241 の反応式
[F:1][C:2]([F:36])([F:35])[C:3]1[CH:4]=[C:5]([CH:28]=[C:29]([C:31]([F:34])([F:33])[F:32])[CH:30]=1)[C:6]([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]#[C:16][CH2:17]Cl)[CH2:10][C@H:9]1[CH2:19][C:20]1[CH:25]=[CH:24][C:23]([CH3:26])=[C:22]([CH3:27])[CH:21]=1)=[O:7].Cl.[CH2:38]([O:40][C:41]([C@@H:43]1[CH2:48][O:47][CH2:46][CH2:45][NH:44]1)=[O:42])[CH3:39].C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CN(C)C=O>[F:1][C:2]([F:36])([F:35])[C:3]1[CH:4]=[C:5]([CH:28]=[C:29]([C:31]([F:34])([F:33])[F:32])[CH:30]=1)[C:6]([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]#[C:16][CH2:17][N:44]2[CH2:45][CH2:46][O:47][CH2:48][C@H:43]2[C:41]([O:40][CH2:38][CH3:39])=[O:42])[CH2:10][C@H:9]1[CH2:19][C:20]1[CH:25]=[CH:24][C:23]([CH3:26])=[C:22]([CH3:27])[CH:21]=1)=[O:7]
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 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 44828818(S)-ethyl morpholine-3-carboxylate hydrochlorideHCID 53806279HCID 53806279、化合物

生成物 1

HCID 57253530HCID 57253530、化合物収率 20.2%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

A mixture of (2R)-1-[3,5-bis(trifluoromethyl)benzoyl]-2-(3,4-dimethylbenzyl)-4-[4-chloro-2-butynyl]piperazine (1.2 g) and (3S)-3-ethoxycarbonylmorpholine hydrochloride (0.43 g), potassium carbonate (1.09 g) and a trace of potassium iodide in N,N-dimethylformamide (50 ml) was stirred at 55° C. for 12 hours. After cooling, the solvent was removed by evaporation, and ethyl acetate and water were added thereto. The organic layer was separated, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by column chromatography on silica gel with a mixture of ethyl acetate and n-hexane (2:3) as an eluent to give (2R)-1-[3,5-bis(trifluoromethyl)benzoyl]-2-(3,4-dimethylbenzyl)-4-[4-((3S)-3-ethoxycarbonylmorpholino)-2-butynyl]piperazine (0.29 g) as an oil.

後処理

  1. temperatureAfter cooling
  2. customthe solvent was removed by evaporation, and ethyl acetate and water
  3. additionwere added
  4. customThe organic layer was separated
  5. dry with materialdried over magnesium sulfate
  6. customevaporated in vacuo
  7. customThe residue was purified by column chromatography on silica gel with a mixture of ethyl acetate and n-hexane (2:3) as an eluent

出典と根拠

ORDレコード
ord-4a822fcec353451ba420705534a97aea
出典データセット
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06924278B2

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