Imidazole → 1-Adamantyl 1-imidazolylmethyl ketone

HRID 259307

反応式

HRID 259307 の反応式
Br[CH2:2][C:3]([C:5]12[CH2:14][CH:9]3[CH2:10][CH:11]([CH2:13][CH:7]([CH2:8]3)[CH2:6]1)[CH2:12]2)=[O:4].CN(C)C=O.[NH:20]1[CH:24]=[CH:23][N:22]=[CH:21]1>O>[NH:20]1[CH:24]=[CH:23][N:22]=[C:21]1[CH2:2][C:3]([C:5]12[CH2:14][CH:9]3[CH2:10][CH:11]([CH2:13][CH:7]([CH2:8]3)[CH2:6]1)[CH2:12]2)=[O:4]

参加物

5

反応物 3

HCID 795ImidazoleHCID 6228Dimethylformamide2 回HCID 197820Bromomethyl tricyclo[3.3.1.13,7]dec-1-yl ketone

生成物 1

HCID 433411781-Adamantyl 1-imidazolylmethyl ketone

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 5 g. of 1-adamantyl bromomethyl ketone in 10 ml. of dimethylformamide is added dropwise with stirring and ice-cooling to 7 g. imidazole in 10 ml. dimethylformamide. The resulting solution is stirred overnight at room temperature and then poured into 250 ml. water. The precipitate which forms is filtered off, washed with water and air dried. Thereafter the resulting residue is chromatographed on silica gel to effect purification. Elution with 10% acetone in dichloromethane yields 1-adamantyl 1-imidazolylmethyl ketone, M.P. 128.5°-129.5° C.

後処理

  1. temperatureice-cooling to 7 g
  2. stirringThe resulting solution is stirred overnight at room temperature
  3. additionpoured into 250 ml
  4. filtrationThe precipitate which forms is filtered off
  5. washwashed with water and air
  6. customdried
  7. customThereafter the resulting residue is chromatographed on silica gel
  8. custompurification
  9. washElution with 10% acetone in dichloromethane

出典と根拠

ORDレコード
ord-b47529ff2e8c445b9a39986abbb92714
出典データセット
uspto-grants-1977_07
特許番号
US04036975

関連ノート

読み込み中…