Dimethylformamide → 6-Chloro-N-{(3S)-1-[(1S)-1-methyl-2-morpholin-4-yl-2-oxoethyl]-2-oxopyrrolidin-3-yl}-N-(2-morpholin-4-ylethyl)naphthalene-2-sulfonamide formate

HRID 33439

반응식

HRID 33439 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([S:12]([NH:15][C@@H:16]1[CH2:20][CH2:19][N:18]([C@H:21]([CH3:29])[C:22]([O:24]C(C)(C)C)=[O:23])[C:17]1=[O:30])(=[O:14])=[O:13])[CH:6]=[CH:5]2.Cl.Cl[CH2:33][CH2:34][N:35]1[CH2:40][CH2:39][O:38][CH2:37][CH2:36]1.C(=O)([O-])[O-].[K+].[K+].[C:47]([O:50][CH2:51][CH3:52])(=O)[CH3:48].C[N:54](C=O)C>O>[CH:22]([OH:24])=[O:23].[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([S:12]([N:15]([C@H:16]1[CH2:20][CH2:19][N:18]([C@@H:21]([CH3:29])[C:22]([N:54]3[CH2:52][CH2:51][O:50][CH2:47][CH2:48]3)=[O:23])[C:17]1=[O:30])[CH2:33][CH2:34][N:35]1[CH2:40][CH2:39][O:38][CH2:37][CH2:36]1)(=[O:13])=[O:14])[CH:6]=[CH:5]2

참가 물질

7

반응물 5

HCID 6228DimethylformamideHCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 77210Morpholine, 4-(2-chloroethyl)-, hydrochloride (1:1)HCID 69222335tert-Butyl(2R)-2-((3R)-3-{[(6-chloro-2-naphthyl)sulfonyl]amino}-2-oxopyrrolidin-1-yl)propanoate

생성물 1

HCID 101893656-Chloro-N-{(3S)-1-[(1S)-1-methyl-2-morpholin-4-yl-2-oxoethyl]-2-oxopyrrolidin-3-yl}-N-(2-morpholin-4-ylethyl)naphthalene-2-sulfonamide formate

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
40 °C

실험 절차

Example 1 (0.05 g) was dissolved in DMF (1 ml) and treated with chloroethylmorpholine hydrochloride (0.062 g) and potassium carbonate (0.093 g), and stirred at 40° C. for 2 h. The mixture was then heated at 80° C. for 8 h, cooled and treated with ethyl acetate and water. The organic extract was dried (over magnesium sulphate) and concentrated under reduced pressure. The residue was purified using mass directed preparative h.p.l.c. to give the title compound (0.018 g) as a white solid.

후처리

  1. temperatureThe mixture was then heated at 80° C. for 8 h
  2. temperaturecooled
  3. extractionThe organic extract
  4. dry with materialwas dried (over magnesium sulphate)
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified

출처 및 근거

ORD 기록
ord-cfcdd9358193486a949f41d25c918519
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429587B2

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