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Diisopropyl Ether → HCID 86745629, 화합물

HRID 1029497
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HRID 1029497 반응식
Cl[CH:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:11])[N:3]1[C:12]1[CH:21]=[CH:20][C:19]2[C:14](=[N:15][C:16]([Cl:22])=[CH:17][CH:18]=2)[N:13]=1.[C:23]([N:28]1[CH2:33][CH2:32][CH:31]([C:34]([OH:36])=[O:35])[CH2:30][CH2:29]1)(=[O:27])[CH2:24][CH2:25][CH3:26].N12CCCN=C1CCCCC2.C(OC(C)C)(C)C>CN(C)C=O>[C:23]([N:28]1[CH2:29][CH2:30][CH:31]([C:34]([O:36][CH:2]2[C:10]3[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=3)[C:4](=[O:11])[N:3]2[C:12]2[CH:21]=[CH:20][C:19]3[C:14](=[N:15][C:16]([Cl:22])=[CH:17][CH:18]=3)[N:13]=2)=[O:35])[CH2:32][CH2:33]1)(=[O:27])[CH2:24][CH2:25][CH3:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 7914Diisopropyl EtherHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 141824043-Chloro-2-(7-chloro-1,8-naphthyridin-2-yl)-1-isoindolinoneHCID 199004171-(1-Oxobutyl)-4-piperidinecarboxylic acid

생성물 1

HCID 86745629HCID 86745629, 화합물수율 40.6%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

The procedure is as in Example 1, but starting with 3-chloro-2-(7-chloro-1,8-naphthyridin-2-yl)-1-isoindolinone (9.9 g) in anhydrous dimethylformamide (100 cc), 1-butyryl-4-piperidinecarboxylic acid (6 g) and 1,8-diazabicyclo[5.4.0]undec-7-ene (4.6 g). The residue obtained is purified by chromatography on silica (0.063-0.2 mm; 250 g) contained in a column 4.2 cm in diameter [eluant: a mixture of methylene chloride and methanol (99:1 by volume)], collecting 70-cc fractions. Fractions 82 to 110 are combined and concentrated to dryness under reduced pressure (b 2.7 kPa). The solid obtained is taken up with stirring with isopropyl ether, then separated by filtration and dried. 2-(7-Chloro-1,8-naphthyridin-2-yl)-3-oxo-1-isoindolinyl 1-butyryl-4-piperidinecarboxylate (6 g), m.p. 165° C., is thereby obtained.

후처리

  1. customThe residue obtained
  2. customis purified by chromatography on silica (0.063-0.2 mm; 250 g)
  3. additiona mixture of methylene chloride and methanol (99:1 by volume)],
  4. customcollecting 70-cc fractions
  5. concentrationconcentrated to dryness under reduced pressure (b 2.7 kPa)
  6. customThe solid obtained
  7. customseparated by filtration
  8. customdried

출처 및 근거

ORD 기록
ord-a06013534be048ab9f8893e57a3f2b94
출처 데이터셋
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05102890

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