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Hydrochloric Acid → HCID 54191570, 화합물

HRID 728105
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HRID 728105 반응식
[Cl-].Cl[CH2:3][C:4](=O)[CH2:5][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[NH2:26][C:27]1[CH:32]=[C:31]([CH3:33])[CH:30]=[CH:29][N:28]=1.[CH2:34]([O:41][C:42]1[CH:43]=[C:44]([CH:47]=[CH:48][C:49]=1[N+:50]([O-:52])=[O:51])[CH:45]=O)[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1.C(=O)([O-])[O-].[K+].[K+].Cl>C(#N)C.O>[CH2:34]([O:41][C:42]1[CH:43]=[C:44]([CH:45]=[CH:5][C:4]2[N:26]=[C:27]3[CH:32]=[C:31]([CH3:33])[CH:30]=[CH:29][N:28]3[CH:3]=2)[CH:47]=[CH:48][C:49]=1[N+:50]([O-:52])=[O:51])[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 15332-Amino-4-methylpyridineHCID 11430Potassium Carbonate2회HCID 27736283-Chloro-2-oxopropyl triphenylphosphonium chlorideHCID 121117193-(Benzyloxy)-4-nitrobenzaldehyde

생성물 1

HCID 54191570HCID 54191570, 화합물수율 45.7%

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

실험 절차

A mixture of (chloroacetonyl)triphenylphosphonium chloride (190.7 g) and 2-amino-4-methylpyridine (158.9 g) in acetonitrile (1.3 l) was stirred under reflux for 5.5 hours. To the reaction mixture were added water (400 ml) and 3-benzyloxy-4-nitrobenzaldehyde (63.0 g) under ice-cooling. The mixture was adjusted to pH 9.5 with potassium carbonate and stirred for 2.5 hours at ambient temperature under keeping the pH 9.5 to 10.0 with 20% aqueous potassium carbonate. The reaction mixture was adjusted to pH 2.0 with conc. hydrochloric acid and the precipitate was collected by filtration. To a mixture of ethyl acetate, tetrahydrofuran and water was added the above obtained precipitate and the resultant mixture was adjusted to pH 7.0 with 20% aqueous potassium carbonate. The separated organic layer was washed with brine and dried over magnesium sulfate. The solvent was removed in vacuo to give 2-[2-(3-benzyloxy-4-nitrophenyl)vinyl]-7-methylimidazo[1,2-a]pyridine (43.14 g).

후처리

  1. temperatureunder reflux for 5.5 hours
  2. temperaturecooling
  3. stirringstirred for 2.5 hours at ambient temperature
  4. filtrationthe precipitate was collected by filtration
  5. additionTo a mixture of ethyl acetate, tetrahydrofuran and water
  6. additionwas added the above obtained precipitate
  7. washThe separated organic layer was washed with brine
  8. dry with materialdried over magnesium sulfate
  9. customThe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-87938e24a82a4465a7dfa21c333e36c3
출처 데이터셋
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05047411

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