Imidazole → 1-Adamantyl 1-imidazolylmethyl ketone

HRID 259307

반응식

HRID 259307 반응식
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]

참가 물질

5

반응물 3

HCID 795ImidazoleHCID 6228Dimethylformamide2회HCID 197820Bromomethyl tricyclo[3.3.1.13,7]dec-1-yl ketone

생성물 1

HCID 433411781-Adamantyl 1-imidazolylmethyl ketone

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b47529ff2e8c445b9a39986abbb92714
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04036975

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