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Diisopropylethylamine → 2-Methyl-4-(1-m-tolyl-1H-[1,2,4]triazole-3-carbonyl)-piperazine-1-carboxylic acid tert-butyl ester

HRID 334076
ノート
印刷プレビュー

反応式

HRID 334076 の反応式
[C:1]1([CH3:15])[CH:6]=[CH:5][CH:4]=[C:3]([N:7]2[CH:11]=[N:10][C:9]([C:12]([OH:14])=O)=[N:8]2)[CH:2]=1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.CCN(C(C)C)C(C)C.[C:47]([O:51][C:52]([N:54]1[CH2:59][CH2:58][NH:57][CH2:56][CH:55]1[CH3:60])=[O:53])([CH3:50])([CH3:49])[CH3:48]>C(Cl)Cl>[C:47]([O:51][C:52]([N:54]1[CH2:59][CH2:58][N:57]([C:12]([C:9]2[N:10]=[CH:11][N:7]([C:3]3[CH:2]=[C:1]([CH3:15])[CH:6]=[CH:5][CH:4]=3)[N:8]=2)=[O:14])[CH2:56][CH:55]1[CH3:60])=[O:53])([CH3:50])([CH3:48])[CH3:49]
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 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 15087784tert-Butyl 2-methylpiperazine-1-carboxylateHCID 713020901-(m-Tolyl)-1H-1,2,4-triazole-3-carboxylic acid

生成物 1

HCID 866882982-Methyl-4-(1-m-tolyl-1H-[1,2,4]triazole-3-carbonyl)-piperazine-1-carboxylic acid tert-butyl ester

試薬・触媒・溶媒

1
HCID 6344Dichloromethane溶媒

実験手順

2.00 g (9.84 mmol) 1-m-tolyl-1H-[1,2,4]-triazole-3-carboxylic acid was stirred with 3.30 g (10.3 mmol) TBTU and 2.50 mL (14.6 mmol) DIPEA in 30 mL DCM at RT. After 10 min, 2.05 g (9.84 mmol) 2-methyl-piperazine-1-carboxylic acid tert-butyl ester was added and the reaction mixture was stirred at RT for 12 h. The solvent was removed by distillation. The residue was taken up in water and extracted with EtOAc. The combined organic phases were dried over sodium sulfate, filtered and concentrated in vacuo. The crude material was purified by flash chromatography (EtOAc).

後処理

  1. customThe solvent was removed by distillation
  2. extractionextracted with EtOAc
  3. dry with materialThe combined organic phases were dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude material was purified by flash chromatography (EtOAc)

出典と根拠

ORDレコード
ord-06ba802c7e5647bfa4f310cb086af794
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08883789B2

反応ノート

読み込み中…

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