Hydrochloric Acid → HCID 178512012、化合物

HRID 659126ノート

反応式

HRID 659126 の反応式
[O:1]1CCCO[CH:2]1[C:7]1[CH:8]=[C:9]([NH:13][C:14]([C:16]2[CH:17]=[C:18]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[CH:19]=[CH:20][C:21]=2[F:22])=[NH:15])[CH:10]=[CH:11][CH:12]=1.Cl.C([O-])(O)=O.[Na+]>C1COCC1>[F:22][C:21]1[CH:20]=[CH:19][C:18]([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=2)=[CH:17][C:16]=1[C:14]([NH:13][C:9]1[CH:10]=[CH:11][CH:12]=[C:7]([CH:2]=[O:1])[CH:8]=1)=[NH:15]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 178512007HCID 178512007、化合物

生成物 1

HCID 178512012HCID 178512012、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To acetal (56) (378 mg) in THF (2 mL) was added 1N hydrochloric acid (2 mL) and the reaction mixture stirred at ambient temperature overnight followed by heating to 50° C. for a further 3 hours. The reaction mixture was cooled to 0° C. and neutralised with saturated NaHCO3 solution. The organics were extracted with EtOAc, dried (MgSO4) and the solvent concentrated in vacuo to give the title compound. Yield: 307 mg, 96%; LC-MS tr 1.26 min; HPLC Purity: 71%; MS (ES+) m/z 319 (M+H)

後処理

  1. temperatureby heating to 50° C. for a further 3 hours
  2. extractionThe organics were extracted with EtOAc
  3. dry with materialdried (MgSO4)
  4. concentrationthe solvent concentrated in vacuo

出典と根拠

ORDレコード
ord-e19e40ad4e0d48dbbf801e1fbba97a7d
出典データセット
uspto-grants-2011_12
特許番号
US08080567B2

反応ノート

読み込み中…