Diisopropylethylamine → [2,2-Dimethyl-4-(3-methylamino-4-nitro-benzoyl)-piperazin-1-yl]-(1-phenyl-1H-[1,2,4]-triazol-3-yl)-methanone

HRID 334072ノート

反応式

HRID 334072 の反応式
FC(F)(F)C(O)=O.[CH3:8][C:9]1([CH3:28])[CH2:14][NH:13][CH2:12][CH2:11][N:10]1[C:15]([C:17]1[N:21]=[CH:20][N:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[N:18]=1)=[O:16].[CH3:29][NH:30][C:31]1[CH:32]=[C:33]([CH:37]=[CH:38][C:39]=1[N+:40]([O-:42])=[O:41])[C:34](O)=[O:35].CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.CCN(C(C)C)C(C)C>CN(C=O)C>[CH3:8][C:9]1([CH3:28])[CH2:14][N:13]([C:34](=[O:35])[C:33]2[CH:37]=[CH:38][C:39]([N+:40]([O-:42])=[O:41])=[C:31]([NH:30][CH3:29])[CH:32]=2)[CH2:12][CH2:11][N:10]1[C:15]([C:17]1[N:21]=[CH:20][N:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[N:18]=1)=[O:16]

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 221846233-(Methylamino)-4-nitrobenzoic acidHCID 86688259(2,2-dimethyl-piperazin-1-yl)-(1-phenyl-1-H-[1,2,4]triazol-3-yl)-methanone trifluoroacetate

生成物 1

HCID 86688294[2,2-Dimethyl-4-(3-methylamino-4-nitro-benzoyl)-piperazin-1-yl]-(1-phenyl-1H-[1,2,4]-triazol-3-yl)-methanone

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 399 mg (1.00 mmol) (2,2-dimethyl-piperazin-1-yl)-(1-phenyl-1-H-[1,2,4]triazol-3-yl)-methanone trifluoroacetate, 196 mg (1.00 mmol) 3-methylamino-4-nitro-benzoic acid, 353 mg (1.10 mmol) TBTU and 600 μL (3.50 mmol) DIPEA in 1.00 mL DMF was stirred at RT for 1 h. The reaction mixture was poured into ice water. The precipitate was filtered off, washed with water and dried.

後処理

  1. filtrationThe precipitate was filtered off
  2. washwashed with water
  3. customdried

出典と根拠

ORDレコード
ord-f786e7b19b824260832496b5d328a140
出典データセット
uspto-grants-2014_11
特許番号
US08883789B2

反応ノート

読み込み中…