Methanesulfonic Acid → HCID 86587635、化合物

HRID 352082

反応式

HRID 352082 の反応式
[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

参加物

5

反応物 2

HCID 6395Methanesulfonic AcidHCID 6444692Mubritinib

生成物 1

HCID 86587635HCID 86587635、化合物収率 98%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

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%).

後処理

  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.)

出典と根拠

ORDレコード
ord-b1868528949c4af58571335dcb643808
出典データセット
uspto-grants-2004_06
特許番号
US06743924B2

関連ノート

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