tert-Butyl piperazine-1-carboxylate → HCID 58899616、化合物

HRID 2246614ノート

反応式

HRID 2246614 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[C:9]([CH:10]=1)=[N:8][N:7]([N+]([O-])=O)[CH:6]=2.[N:14]1([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1>C1COCC1.CN(C1C=CN=CC=1)C.CO>[Br:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([N:17]3[CH2:16][CH2:15][N:14]([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH2:19][CH2:18]3)=[N:7][NH:8]2)=[CH:4][CH:3]=1

参加物

6

反応物 2

HCID 143452tert-Butyl piperazine-1-carboxylate2 回HCID 588996216-bromo-2-nitro-2H-indazole

生成物 1

HCID 58899616HCID 58899616、化合物収率 35.5%

試薬・触媒・溶媒 3

HCID 142844-(Dimethylamino)pyridine触媒HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 6-bromo-2-nitro-2H-indazole (50 mg) and 1,1-dimethylethyl 1-piperazinecarboxylate (107 mg) in THF (1 ml) was stirred at reflux for 18 h. Additional 1,1-dimethylethyl 1-piperazinecarboxylate (107 mg) and DMAP (˜10 mg) were added and heating was continued for 24 h. The mixture was diluted with methanol then purified by reverse phase preparative HPLC to give the title compound as a yellow oil (28 mg).

後処理

  1. temperatureat reflux for 18 h
  2. temperatureheating
  3. customthen purified by reverse phase preparative HPLC

出典と根拠

ORDレコード
ord-898cbbd701274426ae69f02409c35220
出典データセット
uspto-grants-2010_03
特許番号
US07687532B2

反応ノート

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