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Hydrochloric Acid → HCID 57978659, 화합물

HRID 1866862
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HRID 1866862 반응식
[CH3:1]C1C=CC(S(O)(=O)=O)=CC=1.[C:12]1([C:18]2([C:25]3[CH:34]=[C:33]([O:35][CH2:36][C:37]4[CH:46]=[CH:45][C:44]5[C:39](=[CH:40][CH:41]=[CH:42][CH:43]=5)[N:38]=4)[CH:32]=[CH:31][C:26]=3[C:27]([NH:29][NH2:30])=[O:28])[CH2:23][CH:22]3[CH2:24][CH:19]2[CH2:20][CH2:21]3)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.Cl.C(=O)(O)[O-].[Na+]>C(OC(OCC)OCC)C>[O:28]1[CH:1]=[N:30][N:29]=[C:27]1[C:26]1[CH:31]=[CH:32][C:33]([O:35][CH2:36][C:37]2[CH:46]=[CH:45][C:44]3[C:39](=[CH:40][CH:41]=[CH:42][CH:43]=3)[N:38]=2)=[CH:34][C:25]=1[C:18]1([C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH2:23][CH:22]2[CH2:24][CH:19]1[CH2:20][CH2:21]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric Acid2회HCID 6101p-Toluenesulfonic acidHCID 516892Sodium BicarbonateHCID 57978651HCID 57978651, 화합물

생성물 1

HCID 57978659HCID 57978659, 화합물

시약·촉매·용매 1

HCID 31214Ethyl orthoformate용매

실험 절차

A catalytic amount of p-TSA (˜3 mg) was added to a stirred suspension of 4d HCl salt (54.6 mg, 0.10 mmol) in triethylorthoformate (600 μL) at room temperature. After 30 min, 1N hydrochloric acid (600 μL) was added, and the resulting solution was aged for an additional 45 min. The reaction mixture was poured into saturated aqueous sodium bicarbonate and extracted three times with EtOAc. The combined organic extracts were washed with brine, dried (Na2SO4) and concentrated in vacuo. The crude residue was purified by preparative reversed phase HPLC on YMC Pack Pro C18 stationary phase (gradient elution; 0-75% acetonitrile/water as eluent, 0.1% TFA as modifier). Lyophilization of the purified fractions afforded the title compound Sc, m/z (ES) 474 (MH)+.

후처리

  1. waitthe resulting solution was aged for an additional 45 min
  2. extractionextracted three times with EtOAc
  3. washThe combined organic extracts were washed with brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated in vacuo
  6. customThe crude residue was purified by preparative reversed phase HPLC on YMC Pack Pro C18 stationary phase (gradient elution; 0-75% acetonitrile/water as eluent, 0.1% TFA as modifier)

출처 및 근거

ORD 기록
ord-ca94dbd98376458c9bd4b46278dec6fd
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07629467B2

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