Water → Mubritinib

HRID 352070

反応式

HRID 352070 の反応式
[N:1]1([CH2:6][CH2:7][CH2:8][CH2:9][C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)[CH:5]=[CH:4][N:3]=[N:2]1.Cl[CH2:18][C:19]1[N:20]=[C:21](/[CH:24]=[CH:25]/[C:26]2[CH:31]=[CH:30][C:29]([C:32]([F:35])([F:34])[F:33])=[CH:28][CH:27]=2)[O:22][CH:23]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O.CO>[F:35][C:32]([F:33])([F:34])[C:29]1[CH:30]=[CH:31][C:26](/[CH:25]=[CH:24]/[C:21]2[O:22][CH:23]=[C:19]([CH2:18][O:16][C:13]3[CH:12]=[CH:11][C:10]([CH2:9][CH2:8][CH2:7][CH2:6][N:1]4[CH:5]=[CH:4][N:3]=[N:2]4)=[CH:15][CH:14]=3)[N:20]=2)=[CH:27][CH:28]=1

参加物

7

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 9857126HCID 9857126、化合物HCID 121094944-(4-[1,2,3]Triazol-1-yl-butyl)phenol2 回

生成物 1

HCID 6444692Mubritinib収率 93%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

4-[4-(1H-1,2,3-Triazol-1-yl)butyl]phenol (400 mg, 1.84 mmol) and 4-(chloromethyl)-2-[(E)-2-[4-(trifluoromethyl)phenyl]ethenyl]-1,3-oxazole (529 mg, 1.84 mmol) were dissolved in dimethylformamide (3 ml), potassium carbonate (279 mg, 2.02 mmol) was added and the mixture was stirred at 65-75° C. for 4 hours. 4-[4-(1H-1,2,3-Triazol-1-yl)butyl]phenol (40 mg, 0.184 mmol) was added and the mixture was stirred at 65-75° C. for 3 more hours. After cooling to room temperature, water (5 ml) and methanol (3 ml) were added in this order, and the mixture was stirred at room temperature for 40 min. The precipitated crystals were collected by filtration, washed with water and dried under reduced pressure to give 1-[4-[4-[[2-[(E)-2-[-4-(trifiuoromethyl)phenyl]ethenyl]-1,3-oxazol-4-yl]methoxy]phenyl]butyl]-1H-1,2,3-triazole (799 mg, yield 93%).

後処理

  1. stirringthe mixture was stirred at 65-75° C. for 3 more hours
  2. temperatureAfter cooling to room temperature
  3. stirringthe mixture was stirred at room temperature for 40 min
  4. filtrationThe precipitated crystals were collected by filtration
  5. washwashed with water
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-78a8ec52042f4154a67abca99c56a8df
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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