tert-Butyl piperazine-1-carboxylate → HCID 58899616, 화합물

HRID 2246614노트

반응식

HRID 2246614 반응식
[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

참가 물질

6

반응물 2

HCID 143452tert-Butyl piperazine-1-carboxylate2회HCID 588996216-bromo-2-nitro-2H-indazole

생성물 1

HCID 58899616HCID 58899616, 화합물수율 35.5%

시약·촉매·용매 3

HCID 142844-(Dimethylamino)pyridine촉매HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-898cbbd701274426ae69f02409c35220
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07687532B2

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