Hydrochloric Acid → HCID 178512012, 화합물

HRID 659126노트

반응식

HRID 659126 반응식
[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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 178512007HCID 178512007, 화합물

생성물 1

HCID 178512012HCID 178512012, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-e19e40ad4e0d48dbbf801e1fbba97a7d
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08080567B2

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