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Acetic Acid → HCID 86705124, 화합물

HRID 541551
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HRID 541551 반응식
[C:1](=[O:8])([O:5][CH2:6][CH3:7])[O:2][CH2:3]Cl.[Na+].[I-].O=C(C1C=CC=CC=1)C[O:14][C:15](=[O:43])[C@H:16]([OH:42])[CH2:17][N:18]([CH2:28][C:29]1[CH:34]=[CH:33][C:32]([C:35]2[CH:40]=[CH:39][CH:38]=[C:37]([Cl:41])[CH:36]=2)=[CH:31][CH:30]=1)[NH:19][C:20]([C:22]1[O:26][N:25]=[C:24]([OH:27])[CH:23]=1)=[O:21].C(=O)([O-])[O-].[Cs+].[Cs+].CC(O)=O>CC(C)=O.[Zn]>[Cl:41][C:37]1[CH:36]=[C:35]([C:32]2[CH:31]=[CH:30][C:29]([CH2:28][N:18]([CH2:17][C@@H:16]([OH:42])[C:15]([OH:43])=[O:14])[NH:19][C:20]([C:22]3[O:26][N:25]=[C:24]([O:27][CH2:3][O:2][C:1]([O:5][CH2:6][CH3:7])=[O:8])[CH:23]=3)=[O:21])=[CH:34][CH:33]=2)[CH:40]=[CH:39][CH:38]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 176Acetic AcidHCID 5238Sodium IodideHCID 10796Cesium carbonateHCID 5325479Chloromethyl Ethyl CarbonateHCID 178521475HCID 178521475, 화합물

생성물 1

HCID 86705124HCID 86705124, 화합물수율 7.6%

시약·촉매·용매 2

HCID 23994Zinc촉매
HCID 180Acetone용매2회

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온도
60 °C

실험 절차

A mixture of chloromethyl ethyl carbonate (22.7 mg, 164 μmol) and NaI (24.5 mg, 164 μmol) in acetone (2.0 mL, 27 mmol) was stirred at 60° C. for 1 hour, then cooled to room temperature and added to a mixture of (R)-3-[N-(3′-chlorobiphenyl-4-ylmethyl)-N′-(3-hydroxyisoxazole-5-carbonyl)hydrazino]-2-hydroxypropionic acid 2-oxo-2-phenylethyl ester (30.0 mg, 54.5 μmol) and cesium carbonate (17.8 mg, 0.054.5 μmol) in acetone (1 mL). The resulting mixture was stirred at room temperature for 2 hours, concentrated, dissolved in AcOH (2 mL), filtered, and purified by reverse phase preparative HPLC. The desired fractions were combined and concentrated. Zinc (178 mg, 2.7 mmol) and AcOH (1.0 mL, 18 mmol) were added and the resulting mixture was stirred at room temperature for 2 hours. The mixture was filtered and purified by reverse phase preparative HPLC to yield the title compound (2.2 mg). MS m/z [M+H]+ calc'd for C24H24ClN3O9, 534.12. found 534.3.

후처리

  1. temperaturecooled to room temperature
  2. stirringThe resulting mixture was stirred at room temperature for 2 hours
  3. concentrationconcentrated
  4. dissolutiondissolved in AcOH (2 mL)
  5. filtrationfiltered
  6. custompurified by reverse phase preparative HPLC
  7. concentrationconcentrated
  8. stirringthe resulting mixture was stirred at room temperature for 2 hours
  9. filtrationThe mixture was filtered
  10. custompurified by reverse phase preparative HPLC

출처 및 근거

ORD 기록
ord-b805ed5bc36f44faba74f255e66a46f6
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08871792B2

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