Water → Ambrisentan

HRID 1854783

反応式

HRID 1854783 の反応式
[OH:1][C@@H:2]([C:6]([O:19][CH3:20])([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[C:3]([O-:5])=[O:4].Cl[C@H](C1C=CC(Cl)=CC=1)C[NH3+].CC(C)([O-])C.[Na+].[CH3:38][C:39]1[CH:44]=[C:43]([CH3:45])[N:42]=[C:41](S(C)(=O)=O)[N:40]=1.O>CN(C=O)C>[CH3:45][C:43]1[CH:44]=[C:39]([CH3:38])[N:40]=[C:41]([O:1][C@@H:2]([C:6]([O:19][CH3:20])([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[C:3]([OH:5])=[O:4])[N:42]=1

参加物

6

反応物 4

HCID 962WaterHCID 27723824,6-Dimethyl-2-methylsulfonylpyrimidineHCID 23676156Sodium t-butoxideHCID 86668129(R)-2,4-dichlorophenylethyl ammonium (S)-2-hydroxy-3-methoxy-3,3-diphenylpropionate

生成物 1

HCID 6918493Ambrisentan

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

In a 25 mL three neck flask with stirring arrangement, (1 gm) (R)-2,4-dichlorophenylethyl ammonium (S)-2-hydroxy-3-methoxy-3,3-diphenylpropionate and (0.622 gm) sodium tertiary butoxide (6.488 mmol) in 10 ml DMF at 25° C. were taken and stirred for 5 min. (0.604 gm) 4,6-dimethyl-2-(methylsulfonyl)pyrimidine (3.244 mmol) was added to the reaction mixture in one lot. The reaction mixture was stirred at room temperature for 4 hours and subsequently dumped into cold water and aqueous layer was washed with toluene. Aqueous layer was collected and acidified with HCl to adjust pH to 2. Solid white material was precipitated. Solid white material was precipitated. The solid so obtained was filtered, washed with water and dried.

後処理

  1. additionwas added to the reaction mixture in one lot
  2. washwas washed with toluene
  3. customAqueous layer was collected
  4. customSolid white material was precipitated
  5. customSolid white material was precipitated
  6. customThe solid so obtained
  7. filtrationwas filtered
  8. washwashed with water
  9. customdried

出典と根拠

ORDレコード
ord-05d505829b234320a1ec76f18191e8c4
出典データセット
uspto-grants-2015_02
特許番号
US08962832B2

関連ノート

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