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

4-Methylmorpholine → 1-Boc-4-(2-(4-Fluoro-3-(trifluoromethyl)phenyl)-2-oxoethylcarbamoyl)piperidine

HRID 2283945
ノート
印刷プレビュー

反応式

HRID 2283945 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([OH:16])=O)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].CN1CCOCC1.CC(C)CC(Cl)=O.[Cl-].[F:32][C:33]1[CH:38]=[CH:37][C:36]([C:39](=[O:42])[CH2:40][NH3+:41])=[CH:35][C:34]=1[C:43]([F:46])([F:45])[F:44]>C1COCC1>[F:32][C:33]1[CH:38]=[CH:37][C:36]([C:39](=[O:42])[CH2:40][NH:41][C:14]([CH:11]2[CH2:10][CH2:9][N:8]([C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7])[CH2:13][CH2:12]2)=[O:16])=[CH:35][C:34]=1[C:43]([F:44])([F:45])[F:46]
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

6

反応物 4

HCID 79724-MethylmorpholineHCID 66054Isovaleryl chlorideHCID 3928711-(tert-Butoxycarbonyl)-4-piperidinecarboxylic acidHCID 89442701[2-[4-Fluoro-3-(trifluoromethyl)phenyl]-2-oxoethyl]azanium;chloride

生成物 1

HCID 534391291-Boc-4-(2-(4-Fluoro-3-(trifluoromethyl)phenyl)-2-oxoethylcarbamoyl)piperidine収率 71.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-10 °C

実験手順

To a solution of piperidine-1,4-dicarboxylic acid mono-tert-butyl ester (9611.92 mg; 41.92 mmol; 1.08 eq.) in THF 100 ml, added 4-methyl-morpholine (14.51 ml; 131.98 mmol; 3.40 eq.), The reaction mixture was cooled to −10° C., 3-methyl-butyryl chloride (5.03 ml; 38.82 mmol; 1.00 eq.) was add dropwise and maintaining the temperature below −5° C. after stirring for 30 mins at from −5° C. to 10° C., 2-(4-Fluoro-3-trifluoromethyl-phenyl)-2-oxo-ethyl-ammonium chloride (10.00 g; 38.82 mmol; 1.00 eq.) was added at −5° C. and stirred the mixture for 20 mins and then RT for 1 h. Added brine, extracted with EA, washed with brine, dried and concentrated. The crude oil was treated with ether. The white solid was collected as the title compound (12 g, yield 71.5%).

後処理

  1. temperaturemaintaining the temperature below −5° C.
  2. additionwas added at −5° C.
  3. waitRT for 1 h
  4. extractionAdded brine, extracted with EA
  5. washwashed with brine
  6. customdried
  7. concentrationconcentrated
  8. additionThe crude oil was treated with ether

出典と根拠

ORDレコード
ord-ca0a5c2d2eae40bfb4f34a7e278f05b6
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09145392B2

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