1-Methylimidazole → HCID 178480909、化合物

HRID 1422419

反応式

HRID 1422419 の反応式
[CH3:1][N:2]1[CH:6]=[CH:5][N:4]=[CH:3]1.[Cl:7][CH2:8][CH:9]([OH:12])[CH2:10][OH:11]>CO>[Cl-:7].[OH:12][CH:9]([CH2:10][OH:11])[CH2:8][N+:4]1[CH:5]=[CH:6][N:2]([CH3:1])[CH:3]=1

参加物

4

反応物 2

HCID 13901-MethylimidazoleHCID 72903-Chloro-1,2-propanediol

生成物 1

HCID 178480909HCID 178480909、化合物収率 100.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1-Methylimidazole (8.21 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 residue was then dissolved in CH3OH, transferred to a tared flask and concentrated to afford the product as a viscous brown oil (19.3 g, 100%). 1H NMR: δH ppm (400 MHz; DMSO-d6) 3.19-3.29 (m, 1H) 3.36-3.48 (m, 1H) 3.77 (dd, J=6.78, 4.21 Hz, 1H) 3.87 (s, 3H) 4.10 (dd, J=13.74, 7.69 Hz, 1H) 4.32 (dd, J=13.74, 3.11 Hz, 1H) 5.13 (br. s., 1H) 5.53 (d, J=5.13 Hz, 1H) 7.72 (t, J=1.74 Hz, 1H) 7.74 (t, J=1.74 Hz, 1H) 9.18 (s, 1H).

後処理

  1. customtransferred to a tared flask
  2. concentrationconcentrated

出典と根拠

ORDレコード
ord-849f9e6c180c423a86fdd24c6d74c100
出典データセット
uspto-grants-2015_01
特許番号
US08926732B2

関連ノート

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