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Ammonium Chloride → methyl 4-[(E)-3-(1-tritylimidazol-5-yl)prop-1-en-1-yl]-2-(4-fluorophenyl)benzoate

HRID 1019043
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HRID 1019043 반응식
C([Mg]Br)C.[C:5]([N:24]1[C:28](I)=[CH:27][N:26]=[CH:25]1)([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[Cu]C#N.[Cl-].[Li+].Br[CH2:36][CH:37]=[CH:38][C:39]1[CH:48]=[CH:47][C:42]([C:43]([O:45][CH3:46])=[O:44])=[C:41]([C:49]2[CH:54]=[CH:53][C:52]([F:55])=[CH:51][CH:50]=2)[CH:40]=1.[Cl-].[NH4+]>C1COCC1>[C:5]([N:24]1[C:28]([CH2:36]/[CH:37]=[CH:38]/[C:39]2[CH:48]=[CH:47][C:42]([C:43]([O:45][CH3:46])=[O:44])=[C:41]([C:49]3[CH:50]=[CH:51][C:52]([F:55])=[CH:53][CH:54]=3)[CH:40]=2)=[CH:27][N:26]=[CH:25]1)([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1
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참가 물질

8

반응물 6

HCID 25517Ammonium ChlorideHCID 433294Lithium ChlorideHCID 154285835-iodo-1-trityl-1H-imidazoleHCID 54112501Methyl 2-(4-fluorophenyl)-4-(3-bromoprop-1-en-1-yl)benzoateHCID 178418443HCID 178418443, 화합물HCID 178418546HCID 178418546, 화합물

생성물 1

HCID 18399521
methyl 4-[(E)-3-(1-tritylimidazol-5-yl)prop-1-en-1-yl]-2-(4-fluorophenyl)benzoate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

Ethyl magnesium bromide (3M solution in ether; 5.7 ml; 17 mmol) was added dropwise at 0° C. under argon atmosphere to a solution of N-trityl 5-iodoimidazole (6.1 g; 14 mmol). After stirring at 0° C. for 1 hour, a solution of copper (I) cyanide (0.27 g; 3 mmol) and lithium chloride (0.252 g; 6 mmol) in THF (5 ml) was added. The mixture was cooled down to −78° C. and a solution of methyl 4-(3-bromoprop-1-en-1-yl)-2-(4-fluorophenyl)benzoate (3.5 g; 10 mmol) in THF (10 ml) was added. After stirring at −78° C. for 15 minutes, the temperature was allowed to raise to room temperature. The mixture was stirred further overnight. After addition of aqueous ammonium chloride solution and evaporation to dryness, the residue was extracted with dichloromethane/distilled water. The organic layer was evaporated to give methyl 4-[(E)-3-(1-tritylimidazol-5-yl)prop-1-en-1-yl]-2-(4-fluorophenyl)benzoate which was used in the next step without further purification.

후처리

  1. temperatureThe mixture was cooled down to −78° C.
  2. stirringAfter stirring at −78° C. for 15 minutes
  3. temperatureto raise to room temperature
  4. stirringThe mixture was stirred further overnight
  5. extractionthe residue was extracted with dichloromethane/
  6. distillationdistilled water
  7. customThe organic layer was evaporated

출처 및 근거

ORD 기록
ord-51ad9ecd638e4dd8b70f435f8d04fd10
출처 데이터셋
uspto-grants-2002_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06486156B1

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