Dimethylamine → N,N-dimethyl-1-(4-nitrophenyl)piperidine-4-carboxamide

HRID 57574

反応式

HRID 57574 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:15][CH2:14][CH:13]([C:16]([OH:18])=O)[CH2:12][CH2:11]2)=[CH:6][CH:5]=1)([O-:3])=[O:2].[NH:19]([CH3:21])[CH3:20].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C>C1COCC1.O>[CH3:20][N:19]([CH3:21])[C:16]([CH:13]1[CH2:12][CH2:11][N:10]([C:7]2[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:9][CH:8]=2)[CH2:15][CH2:14]1)=[O:18]

参加物

7

反応物 4

HCID 674DimethylamineHCID 81531DiisopropylethylamineHCID 27672651-(4-Nitrophenyl)piperidine-4-carboxylic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)

生成物 1

HCID 16370119N,N-dimethyl-1-(4-nitrophenyl)piperidine-4-carboxamide

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 1-(4-nitrophenyl)piperidine-4-carboxylic acid, (CH3)2NH (2.37 g, 29.06 mmol), HATU (11.05 g, 29.06 mmol) and DIPEA (7.51 g, 58.12 mmol) in 30 mL of THF, was stirred at room temperature overnight. The mixture was added to 20 mL of water, extracted with EA, washed with water and brine, dried over Na2SO4. The volatiles were removed in vacuo to give 4.2 g of N,N-dimethyl-1-(4-nitrophenyl)piperidine-4-carboxamide. MS (m/z)=278 (M+H)+.

後処理

  1. extractionextracted with EA
  2. washwashed with water and brine
  3. dry with materialdried over Na2SO4
  4. customThe volatiles were removed in vacuo

出典と根拠

ORDレコード
ord-50e724b041f8481db32ad1c93d67fdcd
出典データセット
uspto-grants-2016_09
特許番号
US09434726B2

関連ノート

読み込み中…