3-Chloro-1,2-propanediol → HCID 178521461、化合物

HRID 62551

反応式

HRID 62551 の反応式
[CH2:1]([N:8]1[CH:12]=[CH:11][N:10]=[CH:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:13][CH2:14][CH:15]([OH:18])[CH2:16][OH:17]>CO>[Cl-:13].[OH:18][CH:15]([CH2:16][OH:17])[CH2:14][N+:10]1[CH:11]=[CH:12][N:8]([CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH:9]=1

参加物

4

反応物 2

HCID 72903-Chloro-1,2-propanediolHCID 779181-Benzylimidazole

生成物 1

HCID 178521461HCID 178521461、化合物収率 97%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1-Benzylimidazole (3.95 g, 25.0 mmol) and 3-chloro-1,2-propanediol (2.76 g, 25.0 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 and transferred to a tared flask and concentrated to afford the product as a viscous brown oil (6.50 g, 97%). 1H NMR: δH ppm (400 MHz; DMSO-d6) 3.18-3.30 (m, 1H) 3.37-3.49 (m, 1H) 3.73-3.86 (m, 1H) 4.15 (dd, J=13.74, 7.69 Hz, 1H) 4.36 (dd, J=13.74, 3.11 Hz, 1H) 5.21 (t, J=5.50 Hz, 1H) 5.49 (s, 2H) 5.62 (d, J=5.50 Hz, 1H) 7.32-7.50 (m, 5H) 7.80 (t, J=1.83 Hz, 1H) 7.86 (t, J=1.83 Hz, 1H) 9.49 (t, J=1.56 Hz, 1H).

後処理

  1. customtransferred to a tared flask
  2. concentrationconcentrated

出典と根拠

ORDレコード
ord-673cfc799ee74f379d56654ddda1146a
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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