Methanesulfonic Acid → HCID 86587635, 화합물

HRID 352082

반응식

HRID 352082 반응식
[F:1][C:2]([F:34])([F:33])[C:3]1[CH:8]=[CH:7][C:6](/[CH:9]=[CH:10]/[C:11]2[O:12][CH:13]=[C:14]([CH2:16][O:17][C:18]3[CH:23]=[CH:22][C:21]([CH2:24][CH2:25][CH2:26][CH2:27][N:28]4[CH:32]=[CH:31][N:30]=[N:29]4)=[CH:20][CH:19]=3)[N:15]=2)=[CH:5][CH:4]=1.[CH3:35][S:36]([OH:39])(=[O:38])=[O:37]>C(OCC)(=O)C.O1CCCC1>[CH3:35][S:36]([OH:39])(=[O:38])=[O:37].[F:34][C:2]([F:1])([F:33])[C:3]1[CH:4]=[CH:5][C:6](/[CH:9]=[CH:10]/[C:11]2[O:12][CH:13]=[C:14]([CH2:16][O:17][C:18]3[CH:23]=[CH:22][C:21]([CH2:24][CH2:25][CH2:26][CH2:27][N:28]4[CH:32]=[CH:31][N:30]=[N:29]4)=[CH:20][CH:19]=3)[N:15]=2)=[CH:7][CH:8]=1

참가 물질

5

반응물 2

HCID 6395Methanesulfonic AcidHCID 6444692Mubritinib

생성물 1

HCID 86587635HCID 86587635, 화합물수율 98%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

실험 절차

1-[4-[4-[[2-[(E)-2-[4-(Trifluoromethyl)phenyl]ethenyl]-1,3-oxazol-4-yl]methoxy]phenyl]butyl]-1H-1,2,3-triazole (1.0 g) was dissolved in ethyl acetate (50 ml) and tetrahydrofuran (5 ml). A solution of methanesulfonic acid (205 mg) in tetrahydrofuran (5 ml) was added dropwise. The crystals were precipitated. The mixture was stirred at room temperature for 20 min and under ice-cooling for 50 min. The reaction mixture was concentrated under reduced pressure until the liquid amount became about half. After stirring the mixture under ice-cooling for 30 min, the mixture was filtrated, washed with ethyl acetate/isopropyl ether=1/1 (3 ml) and dried under reduced pressure (40° C.) to give 1-[4-[4-[ [2-[ (E)-2-[4-(trifluoromethyl)-phenyl]ethenyl]-1,3-oxazol-4-yl]methoxy]phenyl]butyl]-1H-1,2,3-triazole methanesulfonate (1.18 g, yield 98%).

후처리

  1. customThe crystals were precipitated
  2. temperaturecooling for 50 min
  3. concentrationThe reaction mixture was concentrated under reduced pressure until the liquid amount
  4. stirringAfter stirring the mixture under ice-
  5. temperaturecooling for 30 min
  6. filtrationthe mixture was filtrated
  7. washwashed with ethyl acetate/isopropyl ether=1/1 (3 ml)
  8. customdried under reduced pressure (40° C.)

출처 및 근거

ORD 기록
ord-b1868528949c4af58571335dcb643808
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06743924B2

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