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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 → HCID 67207151、化合物

HRID 1476093
ノート
印刷プレビュー

反応式

HRID 1476093 の反応式
C(OP([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])(OCC)=O)C.[H-].[Na+].[F:17][C:18]([F:32])([F:31])[C:19]([C:21]1[CH:26]=[CH:25][C:24]([F:27])=[C:23]([N+:28]([O-:30])=[O:29])[CH:22]=1)=O.O>C1COCC1.CN(C=O)C>[F:32][C:18]([F:17])([F:31])[C:19]([C:21]1[CH:26]=[CH:25][C:24]([F:27])=[C:23]([N+:28]([O-:30])=[O:29])[CH:22]=1)=[CH:9][C:10]([O:12][CH2:13][CH3:14])=[O:11]
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

7

反応物 4

HCID 962WaterHCID 13345Triethyl phosphonoacetateHCID 24758Sodium hydrideHCID 67207883HCID 67207883、化合物

生成物 1

HCID 67207151HCID 67207151、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
0 °C

実験手順

10.9 g (48.5 mmol) of ethyl diethylphosphonoacetate were slowly added dropwise to an ice-cooled suspension of 1.86 g (60% in mineral oil, 46.4 mmol) of sodium hydride in a mixture of 70 ml of THF and 20 ml of DMF. After the addition had ended, the mixture was stirred at 0° C. for another 30 min, and 10.0 g (42.2 mmol) of 2,2,2-trifluoro-1-(4-fluoro-3-nitrophenyl) ethanone were then added. The reaction mixture was stirred at RT overnight and then added to water. The mixture was extracted three times with ethyl acetate, and the combined organic phases were concentrated under reduced pressure. The crude product gave, after chromatography on silica gel (mobile phase cyclohexane/ethyl acetate 20:1 to 10:1), 9.23 g of the target product (71.2% of theory).

後処理

  1. temperaturecooled
  2. additionAfter the addition
  3. stirringThe reaction mixture was stirred at RT overnight
  4. extractionThe mixture was extracted three times with ethyl acetate
  5. concentrationthe combined organic phases were concentrated under reduced pressure

出典と根拠

ORDレコード
ord-76a37e0c7e57408ab538192fb7434aef
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09018414B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート