5-[2,6-Difluoro-4-(1-hydroxy-1-methylethyl)phenyl]-2-({2-[2-(trimethylsilyl)ethoxy]pyrimidin-4-yl}amino)thiophene-3-carboxamide → HCID 178458580、化合物

HRID 386125ノート

反応式

HRID 386125 の反応式
[F:1][C:2]1[CH:7]=[C:6]([C:8]([OH:11])([CH3:10])[CH3:9])[CH:5]=[C:4]([F:12])[C:3]=1[C:13]1[S:17][C:16]([NH:18][C:19]2[CH:24]=[CH:23][N:22]=[C:21]([O:25]CC[Si](C)(C)C)[N:20]=2)=[C:15]([C:32]([NH2:34])=[O:33])[CH:14]=1>CO.Cl>[F:12][C:4]1[CH:5]=[C:6]([C:8]([OH:11])([CH3:9])[CH3:10])[CH:7]=[C:2]([F:1])[C:3]=1[C:13]1[S:17][C:16]([NH:18][C:19]2[CH:24]=[CH:23][NH:22][C:21](=[O:25])[N:20]=2)=[C:15]([C:32]([NH2:34])=[O:33])[CH:14]=1

参加物

4

反応物 1

HCID 595257675-[2,6-Difluoro-4-(1-hydroxy-1-methylethyl)phenyl]-2-({2-[2-(trimethylsilyl)ethoxy]pyrimidin-4-yl}amino)thiophene-3-carboxamide

生成物 1

HCID 178458580HCID 178458580、化合物

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 887Methanol溶媒

実験手順

5-[2,6-Difluoro-4-(1-hydroxy-1-methylethyl)phenyl]-2-({2-[2-(trimethylsilyl)ethoxy]pyrimidin-4-yl}amino)thiophene-3-carboxamide (109 mg, 0.215 mmol) was stirred in a mixture of MeOH (10 mL) and 2N HCl (6 mL) at room temperature overnight. The solvent was removed in vacuo, saturated NaHCO3 was added and the reaction mixture was extracted with EtOAc (2×). The combined organic extracts were washed with brine, dried over MgSO4, filtered, and concentrated in vacuo. Purification of the residue by reverse phase HPLC (40-100% MeCN—H2O) gave the title compound as a pale yellow solid after triturating in DCM.

後処理

  1. customThe solvent was removed in vacuo, saturated NaHCO3
  2. additionwas added
  3. extractionthe reaction mixture was extracted with EtOAc (2×)
  4. washThe combined organic extracts were washed with brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customPurification of the residue by reverse phase HPLC (40-100% MeCN—H2O)

出典と根拠

ORDレコード
ord-e86f7efe837340108723832947f24601
出典データセット
uspto-grants-2013_02
特許番号
US08367706B2

反応ノート

読み込み中…