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Isatin → HCID 19600971、化合物

HRID 610076
ノート
印刷プレビュー

反応式

HRID 610076 の反応式
[NH:1]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:4](=[O:5])[C:2]1=[O:3].[F:12][C:13]([F:17])([F:16])[CH2:14]I>O>[F:12][C:13]([F:17])([F:16])[CH2:14][N:1]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:4](=[O:5])[C:2]1=[O:3]
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

4

反応物 2

HCID 7054IsatinHCID 677091,1,1-Trifluoro-2-iodoethane

生成物 1

HCID 19600971HCID 19600971、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
55 °C

実験手順

Sodium hydride (8.65 g of a 60% oil dispersion, 0.22 mol) was washed with hexane and suspended in hexamethylphosphoramide (200 mL). Isatin (29.4 g, 0.20 mol)) was added carefully. After the gas evolution subsided, 2,2,2-trifluoroethyl iodide (46.2 g, 0.22 mol) was added and the mixture was heated to 55° C. for 4 hours. The solution was cooled, diluted with water (1 L), and the precipitate was collected. The filtrate was acidified with 6 N HCl and a new precipitate formed and was collected. The combined solids were recrystallized from 95% ethanol. Yield 22.5 g (49%). mp 161-163° C.

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

後処理

  1. washSodium hydride (8.65 g of a 60% oil dispersion, 0.22 mol) was washed with hexane
  2. temperatureThe solution was cooled
  3. customthe precipitate was collected
  4. customa new precipitate formed
  5. customwas collected
  6. customThe combined solids were recrystallized from 95% ethanol

出典と根拠

ORDレコード
ord-75715625ac8c4c20a15efd9d6974e6d7
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05998463

反応ノート

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