Ammonia → HCID 178442466, 화합물

HRID 216348노트

반응식

HRID 216348 반응식
CC1C=CC(S([CH2:11][N+:12]#[C-:13])(=O)=O)=CC=1.[NH3:14].[CH3:15][C:16]([CH3:22])([CH2:20][CH3:21])[CH2:17][CH:18]=O.Cl>CO>[CH3:15][C:16]([CH3:22])([CH2:20][CH3:21])[CH2:17][C:18]1[N:14]=[CH:11][NH:12][CH:13]=1

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 161915Tosylmethyl isocyanideHCID 3724921118993-47-8

생성물 1

HCID 178442466HCID 178442466, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

TosMIC (154 g, 0.9 mol) was added to an ambient temperature, saturated solution of ammonia in methanol (7 L). After stirring at ambient temperature for 1 h, 3,3-dimethylpentanal (ca. 0.6 mol) was added over 20 min. After stirring at reflux for 3 h, the reaction mixture was poured into cold 1 N hydrochloric acid and washed with hexane. The aqueous layer was basified with 10 N aqueous sodium hydroxide and extracted with ether. The combined organic extracts were washed with brine, dried (magnesium sulfate), filtered and concentrated in vacuo. Chromatography over silica eluting with 5-10% methanol/methylene chloride afforded 4-(2,2-dimethylbutyl)-1H-imidazole.

후처리

  1. stirringAfter stirring
  2. temperatureat reflux for 3 h
  3. washwashed with hexane
  4. extractionextracted with ether
  5. washThe combined organic extracts were washed with brine
  6. dry with materialdried (magnesium sulfate)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-573d48c680b94777bb80614644ff0e99
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08193228B2

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