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Diisopropylethylamine → N-(1-methyl-4-piperidyl)-7-nitro-benzo[1,3]dioxole-4-carboxamide

HRID 2234491
ノート
印刷プレビュー

反応式

HRID 2234491 の反応式
[NH2:1][CH:2]1[CH2:7][CH2:6][N:5]([CH3:8])[CH2:4][CH2:3]1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[N+:33]([C:36]1[C:41]2[O:42][CH2:43][O:44][C:40]=2[C:39]([C:45](O)=[O:46])=[CH:38][CH:37]=1)([O-:35])=[O:34].C(N(C(C)C)CC)(C)C>CN(C=O)C>[CH3:8][N:5]1[CH2:6][CH2:7][CH:2]([NH:1][C:45]([C:39]2[C:40]3[O:44][CH2:43][O:42][C:41]=3[C:36]([N+:33]([O-:35])=[O:34])=[CH:37][CH:38]=2)=[O:46])[CH2:3][CH2:4]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 4

HCID 81531DiisopropylethylamineHCID 27375314-Amino-1-methylpiperidineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 219488047-Nitrobenzo[d][1,3]dioxole-4-carboxylic acid

生成物 1

HCID 68682205N-(1-methyl-4-piperidyl)-7-nitro-benzo[1,3]dioxole-4-carboxamide収率 51%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4-Amino-1-methylpiperidine (Fluorochem; 325 mg, 2.84 mmol), HATU (1.09 g, 2.84 mmol) and 7-nitrobenzo[1,3]dioxole-4-carboxylic acid (WO 2003082827; 400 mg, 1.89 mmol) were stirred in DMF (5 mL) and diisopropylethylamine (0.99 ml, 5.68 mmol) added. The mixture was stirred for 2 hours at room temperature. The reaction mixture was loaded on to an SCX column, which was subsequently washed with methanol and eluted with ammonia in methanol. Product containing fractions were concentrated and the solid suspended in methanol and filtered off to yield the title compound as a yellow solid (295 mg, 51%).

後処理

  1. washwas subsequently washed with methanol
  2. washeluted with ammonia in methanol
  3. additionProduct containing fractions
  4. concentrationwere concentrated
  5. filtrationfiltered off

出典と根拠

ORDレコード
ord-eaac18c1bee74422bc4730b858d41712
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07709471B2

反応ノート

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