1,2-Dichloroethane → HCID 178473395, 화합물

HRID 1970425노트

반응식

HRID 1970425 반응식
[C:1]1([N:7]2[C:11](=[O:12])[CH:10]=[C:9]([C:13]([OH:15])=O)[NH:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:16]([O:18][C:19]([N:21]1[CH2:26][CH2:25][N:24]([C:27](=[O:38])[C@@H:28]([NH2:37])[CH2:29][C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31])[CH2:23][CH2:22]1)=[O:20])[CH3:17].C(Cl)CCl>CN(C=O)C.CCN(C(C)C)C(C)C>[CH2:16]([O:18][C:19]([N:21]1[CH2:22][CH2:23][N:24]([C:27](=[O:38])[C@@H:28]([NH:37][C:13]([C:9]2[CH:10]=[C:11]([OH:12])[N:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[N:8]=2)=[O:15])[CH2:29][C:30]([O:32][C:33]([CH3:35])([CH3:34])[CH3:36])=[O:31])[CH2:25][CH2:26]1)=[O:20])[CH3:17]

참가 물질

6

반응물 3

HCID 111,2-DichloroethaneHCID 91673915-oxo-1-phenyl-2,5-dihydro-1H-pyrazole-3-carboxylic acidHCID 668549254-((S)-2-amino-3-tert-butoxycarbonyl-propionyl)-piperazine-1-carboxylic acid ethyl ester

생성물 1

HCID 178473395HCID 178473395, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 81531Diisopropylethylamine용매

실험 절차

To a solution of 6.6 g 1-phenyl-3-carboxy-5-pyrazolone and 10.6 g 4-((S)-2-Amino-3-tert-butoxycarbonyl-propionyl)-piperazine-1-carboxylic acid ethyl ester in 30 ml DMF 4.9 g HOBT, 10.6 ml DIPEA and 6.2 g EDC were added and the reaction mixture was stirred for 16 h at RT. Then the reaction mixture was evaporated, diluted with ethyl acetate and subsequently extracted with aqueous LiCl (4% w/w) and aqueous NaHCO3. The organic layer was dried over MgSO4 and the solvent was removed under reduced pressure. The crude product thus obtained was used in the subsequent reaction.

후처리

  1. customThen the reaction mixture was evaporated
  2. additiondiluted with ethyl acetate
  3. extractionsubsequently extracted with aqueous LiCl (4% w/w) and aqueous NaHCO3
  4. dry with materialThe organic layer was dried over MgSO4
  5. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-04485fe4fd834aaba15378ba2d848e81
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08426420B2

반응 노트

불러오는 중…