Iodoethane → 6-Ethoxy-2,2,3,3,4,4,5,5-octafluorohexanol

HRID 1608900ノート

反応式

HRID 1608900 の反応式
[OH-].[K+].[F:3][C:4]([F:18])([C:7]([F:17])([F:16])[C:8]([F:15])([F:14])[C:9]([F:13])([F:12])[CH2:10][OH:11])[CH2:5][OH:6].[CH2:19](I)[CH3:20]>O>[CH2:19]([O:11][CH2:10][C:9]([F:12])([F:13])[C:8]([F:15])([F:14])[C:7]([F:16])([F:17])[C:4]([F:18])([F:3])[CH2:5][OH:6])[CH3:20]

参加物

5

反応物 3

HCID 6340IodoethaneHCID 14797Potassium HydroxideHCID 1361812,2,3,3,4,4,5,5-Octafluorohexane-1,6-diol

生成物 1

HCID 200827806-Ethoxy-2,2,3,3,4,4,5,5-octafluorohexanol収率 43.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

15.4 g potassium hydroxide was dissolved in 200 ml of deionized water, 62 g of 2,2,3,3,4,4,5,5-octafluorohexane-1,6-diol [prepared essentially as described by I.L. Knunyants, L. Chih-yan and V. V. Shokina, Advances in Chem. (Uspekhi Khimi) 32, Original 1502, Eng. Trans. 461-476 (1963); Translation RSIC-165 (Redstone Information Center)] was added, and the mixture was heated to 90° C. Over a period of one hour, 35.7 g of ethyl iodide was added with rapid stirring to the flask via an addition funnel. The reaction mixture was then heated to reflux for two hours. The reaction mixture was cooled to room temperature, and the bottom product phase (54 g crude product) was split away from the aqueous layer. The crude product was distilled at 92°-100° C. at 5.5 mm Hg (5.5 torr) to give 29.1 g of 6-ethoxy-2,2,3,3,4,4,5,5-octafluorohexanol.

後処理

  1. additionTranslation RSIC-165 (Redstone Information Center)] was added
  2. temperatureThe reaction mixture was then heated
  3. temperatureto reflux for two hours
  4. temperatureThe reaction mixture was cooled to room temperature
  5. customthe bottom product phase (54 g crude product) was split away from the aqueous layer
  6. distillationThe crude product was distilled at 92°-100° C. at 5.5 mm Hg (5.5 torr)

出典と根拠

ORDレコード
ord-9b26fa0c5e3143128ab4b9733df0593f
出典データセット
uspto-grants-1995_03
特許番号
US05399291

反応ノート

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