3-Chloro-1,2-propanediol → HCID 178432779、化合物

HRID 62547

反応式

HRID 62547 の反応式
[CH3:1][N:2]1[CH:6]=[CH:5][N:4]=[C:3]1[CH3:7].[Cl:8][CH2:9][CH:10]([OH:13])[CH2:11][OH:12]>CCOCC>[Cl-:8].[OH:13][CH:10]([CH2:11][OH:12])[CH2:9][N+:4]1[CH:5]=[CH:6][N:2]([CH3:1])[C:3]=1[CH3:7]

参加物

4

反応物 2

HCID 72903-Chloro-1,2-propanediolHCID 156171,2-Dimethylimidazole

生成物 1

HCID 178432779HCID 178432779、化合物収率 100%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

1,2-Dimethylimidazole (9.61 g, 100 mmol) and 3-chloro-1,2-propanediol (11.05 g, 100.0 mmol) were stirred in a 130° C. oil bath for 48 h, after which the flask was placed under vacuum and stirring continued at 130° C. for another 48 h. The product was then stirred in refluxing ether for 24 h and filtered to afford a brown solid (20.29 g, 100%). 1H NMR: δH ppm (400 MHz; DMSO-d6) 2.60 (s, 3H) 3.20-3.33 (m, 1H) 3.36-3.49 (m, 2H) 3.78 (s, 3H) 4.08 (dd, J=14.11, 7.88 Hz, 1H) 4.27 (dd, J=14.11, 3.11 Hz, 1H) 5.14 (t, J=5.50 Hz, 1H) 5.50 (d, J=5.68 Hz, 1H) 7.63 (d, J=2.01 Hz, 1H) 7.66 (d, J=2.20 Hz, 1H).

後処理

  1. stirringThe product was then stirred
  2. filtrationfiltered

出典と根拠

ORDレコード
ord-ec93ca77e0d04cc08c1e1fb3ab5ab7ed
出典データセット
uspto-grants-2016_09
特許番号
US09446348B2

関連ノート

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