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tert-Butyl piperazine-1-carboxylate → HCID 10311729, 화합물

HRID 982667
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HRID 982667 반응식
[N:1]1([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.I[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][C:20]1[C:21](=[O:39])[N:22]([C:27]2[CH:34]=[CH:33][C:30]([C:31]#[N:32])=[C:29]([C:35]([F:38])([F:37])[F:36])[CH:28]=2)[C:23](=[O:26])[C:24]=1[CH3:25]>O1CCCC1.C(OCC)(=O)C>[C:31]([C:30]1[CH:33]=[CH:34][C:27]([N:22]2[C:23](=[O:26])[C:24]([CH3:25])=[C:20]([CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][N:4]3[CH2:5][CH2:6][N:1]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:2][CH2:3]3)[C:21]2=[O:39])=[CH:28][C:29]=1[C:35]([F:38])([F:37])[F:36])#[N:32]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 143452tert-Butyl piperazine-1-carboxylateHCID 11306064HCID 11306064, 화합물

생성물 1

HCID 10311729HCID 10311729, 화합물수율 98%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

1.56 g of 1,1-dimethylethyl piperazine-1-carboxylate was added under a nitrogen atmosphere to a solution of 2.0 g of 4-[2,5-dihydro-3-(5-iodopentyl)-4-methyl-2,5-dioxo-1H-pyrrol-1-yl]-2-(trifluoromethyl)benzonitrile in 53 ml of tetrahydrofuran, and this mixture was stirred for 7 days at room temperature. For working-up, it was diluted with ethyl acetate and washed with semi-saturated sodium bicarbonate solution. After drying on sodium sulfate and concentration by evaporation, it was chromatographed with methanol/dichloromethane on silica gel, and thus 2.2 g of the title compound was obtained as a yellowish oil.

후처리

  1. washwashed with semi-saturated sodium bicarbonate solution
  2. customAfter drying on sodium sulfate and concentration by evaporation, it
  3. customwas chromatographed with methanol/dichloromethane on silica gel

출처 및 근거

ORD 기록
ord-38302ad442fa425aa5a6a09044f4f65f
출처 데이터셋
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06861432B2

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