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HCID 66818527, 화합물 → HCID 66818689, 화합물

HRID 1024771
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HRID 1024771 반응식
[CH2:1]([O:3][C:4]([N:6]1[CH2:11][CH2:10][N:9]([C:12](=[O:29])[C:13]2[CH:18]=[C:17]([OH:19])[CH:16]=[C:15]([O:20][C:21]3[CH:26]=[CH:25][C:24]([C:27]#[N:28])=[CH:23][CH:22]=3)[CH:14]=2)[CH2:8][CH2:7]1)=[O:5])[CH3:2]>[Ni].N>[CH2:1]([O:3][C:4]([N:6]1[CH2:11][CH2:10][N:9]([C:12](=[O:29])[C:13]2[CH:18]=[C:17]([OH:19])[CH:16]=[C:15]([O:20][C:21]3[CH:26]=[CH:25][C:24]([CH2:27][NH2:28])=[CH:23][CH:22]=3)[CH:14]=2)[CH2:8][CH2:7]1)=[O:5])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 66818527HCID 66818527, 화합물

생성물 1

HCID 66818689HCID 66818689, 화합물수율 79.5%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 222Ammonia용매

실험 절차

Raney nickel (0.1 g, 1.7 mmols) was added to a stirred solution of 4-[3-(4-cyano phenoxy)-5-hydroxy benzoyl]piperazine-1-carboxylic acid ethyl ester (0.5 g, 1.26 mmols) dissolved in methanolic ammonia (50 ml) and the reaction mixture was heated to 50° C. in Paar apparatus under 50 Psi hydrogen gas pressure for 3 h. The reaction mixture was cooled and filtered through celite pad. The filtrate was concentrated to afford 0.4 g of the required product which was used for the next step without further purification. Percentage purity (LCMS): 74.3%, (M+1)=399.1+1.

후처리

  1. temperatureThe reaction mixture was cooled
  2. filtrationfiltered through celite pad
  3. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-5ba1d5c895c747689928901e12408f85
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08722930B2

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