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Diisopropylethylamine → HCID 9864043, 화합물

HRID 2116448
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HRID 2116448 반응식
Cl[C:2]1[N:10]=[C:9](S(CCC)(=O)=O)[N:8]=[C:7]2[C:3]=1[N:4]=[CH:5][N:6]2[C:17]1[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][CH:18]=1.[NH:24]1[CH2:31][CH2:30][CH2:29][C@H:25]1[C:26]([NH2:28])=[O:27].[CH:32]([N:35](CC)C(C)C)(C)C>O1CCCC1>[Cl:23][C:20]1[CH:19]=[CH:18][C:17]([N:6]2[CH:5]=[N:4][C:3]3[C:7]2=[N:8][C:9]([C:32]#[N:35])=[N:10][C:2]=3[N:24]2[CH2:31][CH2:30][CH2:29][C@H:25]2[C:26]([NH2:28])=[O:27])=[CH:22][CH:21]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 111306L-ProlinamideHCID 85908161HCID 85908161, 화합물

생성물 1

HCID 9864043HCID 9864043, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
90 °C

실험 절차

A solution of the product from step (iii) (0.2 g), L-prolinamide (0.062 g) and N,N-diisopropylethylamine (0.19 ml) in tetrahydrofuran (10 ml) was stirred at room temperature for 24 h. The solvent was removed, the residue dissolved in N,N-dimethylformamide (10 ml) and sodium cyanide (0.05 g) added and heated at 90° C. for 10 h. The mixture was partitioned between ethyl acetate and water, the organics dried (MgSO4) and evaporated under reduced pressure. The residue was purified by RPHPLC. Yield 0.062 g

후처리

  1. customThe solvent was removed
  2. dissolutionthe residue dissolved in N,N-dimethylformamide (10 ml)
  3. additionsodium cyanide (0.05 g) added
  4. customThe mixture was partitioned between ethyl acetate and water
  5. dry with materialthe organics dried (MgSO4)
  6. customevaporated under reduced pressure
  7. customThe residue was purified by RPHPLC

출처 및 근거

ORD 기록
ord-552af0a54c404bacbbf114eed1eb6279
출처 데이터셋
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07439240B2

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