Ammonium Chloride → 2-Di-n-propylamino-8-[2[(isopropylideneamino)oxy]benzoyl]-1,2,3,4-tetrahydronaphthalene

HRID 22141

反応式

HRID 22141 の反応式
[CH3:1][C:2](=[N:4][OH:5])[CH3:3].CC(C)([O-])C.[K+].[CH2:12]([N:15]([CH2:35][CH2:36][CH3:37])[CH:16]1[CH2:25][CH2:24][C:23]2[C:18](=[C:19]([C:26](=[O:34])[C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=3F)[CH:20]=[CH:21][CH:22]=2)[CH2:17]1)[CH2:13][CH3:14].[Cl-].[NH4+]>C1COCC1>[CH2:35]([N:15]([CH2:12][CH2:13][CH3:14])[CH:16]1[CH2:25][CH2:24][C:23]2[C:18](=[C:19]([C:26](=[O:34])[C:27]3[CH:28]=[CH:29][CH:30]=[CH:31][C:32]=3[O:5][N:4]=[C:2]([CH3:3])[CH3:1])[CH:20]=[CH:21][CH:22]=2)[CH2:17]1)[CH2:36][CH3:37]

参加物

6

反応物 4

HCID 25517Ammonium ChlorideHCID 67180Acetone, oximeHCID 152335372-Di-n-propylamino-8-(2'-fluorobenzoyl)-1,2,3,4-tetrahydronaphthaleneHCID 23665647Potassium tert-butoxide

生成物 1

HCID 233735352-Di-n-propylamino-8-[2[(isopropylideneamino)oxy]benzoyl]-1,2,3,4-tetrahydronaphthalene収率 142%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To 47.5 mg of acetone oxime (0.65 mmol) in 25 ml of THF were added 73 mg (0.65 mmol) of potassium t-butoxide. The mixture was stirred at room temperature for one hour after which 210 mg of 2-di-n-propylamino-8-(2'-fluorobenzoyl)-1,2,3,4-tetrahydronaphthalene in THF were added via a syringe. The resulting mixture was refluxed for three hours after which it was cooled and poured into an aqueous solution of ammonium chloride. The mixture then was extracted with either, and the extract was dried and concentrated to obtain 343 mg of 2-di-n-propylamino-8-[2[(isopropylideneamino)oxy]benzoyl]-1,2,3,4-tetrahydronaphthalene.

後処理

  1. additionwere added via a syringe
  2. temperatureThe resulting mixture was refluxed for three hours after which it
  3. temperaturewas cooled
  4. extractionThe mixture then was extracted with either, and the extract
  5. customwas dried
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-2797a14d786349d188da8e5caf5462a1
出典データセット
uspto-grants-1995_06
特許番号
US05426226

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