Hydrochloric Acid → HCID 86651355、化合物

HRID 39496

反応式

HRID 39496 の反応式
[Cl:1][CH:2]([CH2:6][OH:7])[C:3]([OH:5])=[O:4].[F:8][C:9]([F:35])([C:13]([F:34])([F:33])[C:14]([F:32])([F:31])[C:15]([F:30])([F:29])[C:16]([F:28])([F:27])[C:17]([F:26])([F:25])[C:18]([F:24])([F:23])[C:19]([F:22])([F:21])[F:20])[CH2:10][CH2:11]O.Cl>C(OCC)C>[F:8][C:9]([F:35])([C:13]([F:33])([F:34])[C:14]([F:31])([F:32])[C:15]([F:29])([F:30])[C:16]([F:27])([F:28])[C:17]([F:25])([F:26])[C:18]([F:24])([F:23])[C:19]([F:22])([F:21])[F:20])[CH2:10][CH2:11][O:4][C:3](=[O:5])[CH:2]([Cl:1])[CH2:6][OH:7]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 696191,1,2,2-Tetrahydroperfluoro-1-decanolHCID 5649512-Chloro-3-hydroxypropionic acid

生成物 1

HCID 86651355HCID 86651355、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
65 °C

実験手順

In a 50 mL RB with a condenser, 2-chloro-3-hydroxypropionic acid (6.0 g, 0.05 mol) and 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro-1-decanol (18.0 g, 0.04 mol) and a catalytic amount of hydrochloric acid were taken together and heated up to 65° C. for 36 h. Product was dissolved in 300 mL of ethyl ether and washed twice with 100 mL of dil. NaHCO3 aq. sol. and once with 100 mL of sat. aq. NaCl sol. and then dried over anhy. Na2SO4. Solution was filtered, solvent was removed by rotary evaporation and unreacted alcohol was sublimed off at 70° C. under vacuum. Yield=15.0 g (67%). 1H-NMR (CDCl3, 7.27 ppm): 2.54 (m, —CH2CF2). 3.05-3.35 (broad, —OH), 4.01 (m, —CH2OH), 4.42 (m, —CHCl), 4.52 (m, —CO2CH2CH2).

後処理

  1. washwashed twice with 100 mL of dil. NaHCO3 aq. sol. and once with 100 mL of sat. aq. NaCl sol.
  2. customdried over anhy
  3. filtrationSolution was filtered
  4. customsolvent was removed by rotary evaporation and unreacted alcohol
  5. customwas sublimed off at 70° C. under vacuum

出典と根拠

ORDレコード
ord-677c3e9dab1e457ca7d7d2c5e85e43ce
出典データセット
uspto-grants-2013_09
特許番号
US08524942B2

関連ノート

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