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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
ノート
印刷プレビュー

反応式

HRID 1019043 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 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、化合物HCID 178418546HCID 178418546、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-51ad9ecd638e4dd8b70f435f8d04fd10
出典データセット
uspto-grants-2002_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06486156B1

反応ノート

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