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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Water → 2-Oxopropyl [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate

HRID 223824
ノート
印刷プレビュー

反応式

HRID 223824 の反応式
C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[C:20]([Cl:21])=[C:19]([O:22][CH2:23][C:24]([OH:26])=[O:25])[CH:18]=[C:17]2[C:9]=1[C:10]1[C:15]([CH2:27][CH3:28])([CH2:16]2)[CH2:14][CH2:13][C:12](=[O:29])[CH:11]=1.Cl[CH2:31][C:32](=[O:34])[CH3:33].O>CN(C)C=O.CCOCC>[Cl:7][C:8]1[C:20]([Cl:21])=[C:19]([O:22][CH2:23][C:24]([O:26][CH2:31][C:32](=[O:34])[CH3:33])=[O:25])[CH:18]=[C:17]2[C:9]=1[C:10]1[C:15]([CH2:27][CH3:28])([CH2:16]2)[CH2:14][CH2:13][C:12](=[O:29])[CH:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 6571ChloroacetoneHCID 11430Potassium CarbonateHCID 12806939[(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid

生成物 1

HCID 128069492-Oxopropyl [(5,6-Dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetate

試薬・触媒・溶媒 2

HCID 3283
Diethyl Ether
溶媒
HCID 6228Dimethylformamide溶媒

実験手順

Potassium carbonate (0.2 g) is suspended in a solution of [(5,6-dichloro-9a-ethyl-3-oxo-1,2,9,9a-tetrahydro-3H-fluoren-7-yl)oxy]acetic acid (Example 20, Step D) (0.4 g, 0.0011 mole) in dimethylformamide (3 ml). After warming the suspension on a steam bath for 15 minutes, chloroacetone (0.5 g, 0.005 mole) is added and the mixture heated for an additional 15 minutes. The reaction mixture is cooled, poured into water (50 ml) and the product extracted into ether (three 15 ml portions. The extract is dried over Na2SO4. After filtration, the extract is concentrated to give a yellow oil. Trituration with cold ether causes crystallization to occur. The crystalline product weighs 0.1 g and melts at 153°-155° C.

後処理

  1. temperatureAfter warming the suspension on a steam bath for 15 minutes
  2. temperaturethe mixture heated for an additional 15 minutes
  3. temperatureThe reaction mixture is cooled
  4. extractionthe product extracted into ether (three 15 ml portions
  5. dry with materialThe extract is dried over Na2SO4
  6. filtrationAfter filtration
  7. concentrationthe extract is concentrated
  8. customto give a yellow oil
  9. customcrystallization

出典と根拠

ORDレコード
ord-8f447d692b67467f830060e4703da3e5
出典データセット
uspto-grants-1982_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04356314

反応ノート

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