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Diisopropylethylamine → HCID 86590128, 화합물

HRID 1840514
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HRID 1840514 반응식
[NH2:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][C@H:11]([NH:15][C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[C:12]([OH:14])=O)=[CH:4][CH:3]=1.Cl.[CH2:24]([CH:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1)[CH3:25].C(N(CC)C(C)C)(C)C>ClCCl.CN(C)C=O.C(OCC)(=O)C>[NH2:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][C@H:11]([NH:15][C:16](=[O:17])[O:18][C:19]([CH3:22])([CH3:21])[CH3:20])[C:12]([CH:27]2[CH:26]([CH2:24][CH3:25])[CH2:31][CH2:30][NH:29][CH2:28]2)=[O:14])=[CH:4][CH:3]=1
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참가 물질

7

반응물 3

HCID 81531DiisopropylethylamineHCID 15521219HCID 15521219, 화합물HCID 234481304-Ethylpiperidine hydrochloride

생성물 1

HCID 86590128HCID 86590128, 화합물수율 74%

시약·촉매·용매 3

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane
용매
HCID 8857Ethyl Acetate용매

실험 절차

2.1 g (5.5 mmol) of O-(benzotriazol-1l-yl)-N,N,N′, N′-tetramethyluronium hexafluorophosphate (HBTU) are added portionwise with stirring, at 0° C. under nitrogen, to a mixture of 2.0 g of (S)-6-amino-α-[[(1,1-dimethylethoxy)carbonyl]amino]pyridine-3-pentanoic acid (5.5 mmol), 1.14 g (7.5 mmol) of 4-ethylpiperidine hydrochloride, N,N-diisopropylethylamine (DIEA) (25 ml; 14 mmol) in dichloromethane (30 ml) and 3 ml of anhydrous dimethylformamide (DMF). The mixture is allowed to warm to room temperature and stirring is continued for 18 hours. The reaction mixture is taken up in 250 ml of ethyl acetate and is washed with 50 ml of 0.1 N hydrochloric acid solution and with 50 ml of saturated sodium hydrogen carbonate solution and with 50 ml of saturated sodium chloride solution. The product obtained is then dried over sodium sulphate and then filtered and concentrated under reduced pressure. The residue obtained is purified by chromatography on a column of silica gel, eluting under pressure with ethyl acetate. 1.48 g of 1,1-dimethylethyl (S)-[4-(6-aminopyrid-3-yl)-1-([4-ethylpiperid-3-yl)carbonyl]butyl]carbamate are obtained in the form of a viscous oil.

후처리

  1. washis washed with 50 ml of 0.1 N hydrochloric acid solution and with 50 ml of saturated sodium hydrogen carbonate solution and with 50 ml of saturated sodium chloride solution
  2. customThe product obtained
  3. dry with materialis then dried over sodium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue obtained
  7. customis purified by chromatography on a column of silica gel
  8. washeluting under pressure with ethyl acetate

출처 및 근거

ORD 기록
ord-6ac29599a062460e866f808389068838
출처 데이터셋
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06680329B2

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