Imidazole → HCID 69735309、化合物

HRID 496421

反応式

HRID 496421 の反応式
[NH:1]1[CH:5]=[CH:4][N:3]=[CH:2]1.N1C=CC=CC=1.[CH2:12]1[O:20][C@@H:13]1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>C(O)C>[NH:1]1[CH:5]=[CH:4][N:3]=[C:2]1[CH2:12][C@H:13]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[OH:20]

参加物

5

反応物 3

HCID 795ImidazoleHCID 1049PyridineHCID 114705(+)-Styrene oxide

生成物 1

HCID 69735309HCID 69735309、化合物収率 32%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In a manner similar to that of Example 49, step 1, imidazole (2.83 g, 41.6 mmol) is dissolved in absolute ethanol (45 mL). Pyridine (0.11 mL) is added followed by addition of (R)-(+) styrene oxide (5.0 g, 41.6 mol, Aldrich Chemical Co.), followed by heating at reflux for 18 hours. The mixture is evaporated in vacuo to a syrup and suspended between ethyl ether (250 mL) and water (100 mL) to give a solid precipitate. The suspension is filtered and washed with ethyl ether. The solid is recrystallized from hot ethyl acetate and dried in vacuo (2.52 g, 32% yield). MS: APCI: M+1, 189.1 (M: 188.2). NMR spectrum is consistent with structure.

後処理

  1. temperatureby heating
  2. temperatureat reflux for 18 hours
  3. customThe mixture is evaporated in vacuo to a syrup
  4. customto give a solid precipitate
  5. filtrationThe suspension is filtered
  6. washwashed with ethyl ether
  7. customThe solid is recrystallized from hot ethyl acetate
  8. customdried in vacuo (2.52 g, 32% yield)

出典と根拠

ORDレコード
ord-150e80cf7b2f4adaa9053a82b1eba305
出典データセット
uspto-grants-2005_09
特許番号
US06943183B2

関連ノート

読み込み中…