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Acetic Acid → HCID 20148928、化合物

HRID 569302
ノート
印刷プレビュー

反応式

HRID 569302 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 176Acetic AcidHCID 682631,1'-CarbonyldiimidazoleHCID 14098158HCID 14098158、化合物

生成物 1

HCID 20148928HCID 20148928、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2bbe6679334a4545bbddd3661a507455
出典データセット
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04731471

反応ノート

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