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2-Hydroxyisobutyric acid → HCID 53668099、化合物

HRID 569309
ノート
印刷プレビュー

反応式

HRID 569309 の反応式
[C:1]([O:4][CH2:5][CH2:6][C:7]12[CH2:19][CH2:18][C:17](=[O:20])[CH:16]=[C:15]1[C:14]1[C:9](=[CH:10][C:11]([O:23][CH2:24][C:25]([OH:27])=[O:26])=[C:12]([Cl:22])[C:13]=1[Cl:21])[CH2:8]2)(=[O:3])[CH3:2].C(N1C=CN=C1)(N1C=CN=C1)=O.O[C:41]([CH3:46])([CH3:45])[C:42]([OH:44])=[O:43]>O1CCCC1>[C:1]([O:4][CH2:5][CH2:6][C:7]12[CH2:19][CH2:18][C:17](=[O:20])[CH:16]=[C:15]1[C:14]1[C:9](=[CH:10][C:11]([O:23][CH2:24][C:25]([O:27][C:41]([C:42]([OH:44])=[O:43])([CH3:46])[CH3:45])=[O:26])=[C:12]([Cl:22])[C:13]=1[Cl:21])[CH2:8]2)(=[O:3])[CH3:2]
参加物反応条件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 116712-Hydroxyisobutyric acidHCID 682631,1'-CarbonyldiimidazoleHCID 20148928HCID 20148928、化合物

生成物 1

HCID 53668099HCID 53668099、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
20 °C

実験手順

{[9a-(Acetoxyethyl)-5,6-dichloro-3-oxo-2,3,9,9a-tetrahydro-1H-fluoren-7-yl]oxy}acetic acid (4.13 g, 10 mMole) is dissolved in dry tetrahydrofuran (20 ml). 1,1'-Carbonyldiimidazole (3.2 g, 10 mMole) is added and the mixture stirred at 20° C. for an hour. 2-Hydroxy-2-methylpropionic acid (1.05 g, 10 mMole) is added and the mixture stirred for 18 hours at 20° C. The solvent is removed by evaporation in vacuo. The residue is dissolved in methylene chloride, washed with water and dried over MgSO4. The solvent is removed by evaporation in vacuo and the residue purified by chromatography using a silica gel column with methylene chloride/tetrahydrofuran/acetic acid 100/2/1 (V.V.V.) as the eluent. Selecting the appropriate cuts gave the desired compound upon evaporation of the solvent in vacuo.

後処理

  1. stirringthe mixture stirred for 18 hours at 20° C
  2. customThe solvent is removed by evaporation in vacuo
  3. dissolutionThe residue is dissolved in methylene chloride
  4. washwashed with water
  5. dry with materialdried over MgSO4
  6. customThe solvent is removed by evaporation in vacuo
  7. customthe residue purified by chromatography

出典と根拠

ORDレコード
ord-127353321aa74dda8d5621238af7e372
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

読み込み中…

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