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Acetic Acid → HCID 20148928, 화합물

HRID 569302
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HRID 569302 반응식
[C:1]([OH:4])(=[O:3])[CH3:2].C(N1C=CN=C1)(N1C=CN=C1)=O.[Cl:17][C:18]1[C:30]([Cl:31])=[C:29]([O:32][CH2:33][C:34]([OH:36])=[O:35])[CH:28]=[C:27]2[C:19]=1[C:20]1[C:25]([CH2:37][CH2:38]O)([CH2:26]2)[CH2:24][CH2:23][C:22](=[O:40])[CH:21]=1>O1CCCC1>[C:1]([O:4][CH2:38][CH2:37][C:25]12[CH2:24][CH2:23][C:22](=[O:40])[CH:21]=[C:20]1[C:19]1[C:27](=[CH:28][C:29]([O:32][CH2:33][C:34]([OH:36])=[O:35])=[C:30]([Cl:31])[C:18]=1[Cl:17])[CH2:26]2)(=[O:3])[CH3:2]
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참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 682631,1'-CarbonyldiimidazoleHCID 14098158HCID 14098158, 화합물

생성물 1

HCID 20148928HCID 20148928, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of dry tetrahydrofuran (50 ml) containing acetic acid (6.6 mg, 11 mMole) is treated with 1,1'-carbonyldiimidazole (178 mg; 11 mMole) and the mixture stirred under anhydrous conditions for 30 minutes. {[5,6-Dichloro-9a-(2-hydroxyethyl)-3-oxo-2,3,9,9a-tetrahydro-1H-fluoren-7-yl]oxy}acetic acid (3.71 g, 10 mMole) is added and the mixture stirred for 16 hours. The solvent is removed by evaporation at reduced pressure. The residue is dissolved in methylene chloride, treated with 11 mM of HCl, washed with water, and dried over MgSO4. The solvent is removed by evaporation at reduced pressure to give the desired product which is recrystallized from acetonitrile.

후처리

  1. stirringthe mixture stirred for 16 hours
  2. customThe solvent is removed by evaporation at reduced pressure
  3. dissolutionThe residue is dissolved in methylene chloride
  4. additiontreated with 11 mM of HCl
  5. washwashed with water
  6. dry with materialdried over MgSO4
  7. customThe solvent is removed by evaporation at reduced pressure

출처 및 근거

ORD 기록
ord-2bbe6679334a4545bbddd3661a507455
출처 데이터셋
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04731471

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