Hydrochloric Acid → HCID 21697102、化合物

HRID 379039

反応式

HRID 379039 の反応式
C[O:2][C:3](=O)[C:4]1[CH:9]=[CH:8][C:7]([I:10])=[C:6]([O:11][C:12]2[CH:21]=[CH:20][C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[CH:13]=2)[CH:5]=1.[Li+].[BH4-].O.Cl>C1COCC1>[I:10][C:7]1[CH:8]=[CH:9][C:4]([CH2:3][OH:2])=[CH:5][C:6]=1[O:11][C:12]1[CH:21]=[CH:20][C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH:13]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 4148881Lithium borohydrideHCID 539211574-Iodo-3-(naphthalen-2-yloxy)-benzoic acid methyl ester

生成物 1

HCID 21697102HCID 21697102、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

4-Iodo-3-(naphthalen-2-yloxy)-benzoic acid methyl ester (0.10 g, 0.25 mmol) dissolved in THF (2 mL) was treated with LiBH4 (2 M solution in THF) (0.247 mL, 0.495 mmol) and heated at reflux for 1.5 hr. The reaction mixture was cooled, added to H2O (50 mL)- concd HCl (4.3 mL), and extracted with EtOAc (3×30 mL). The organics were combined, washed with H2O, aq saturated NaHCO3 solution, brine, and dried (Na2SO4). Filtration and concentration to dryness gave the title compound which was used without purification.

後処理

  1. temperatureheated
  2. temperatureat reflux for 1.5 hr
  3. temperatureThe reaction mixture was cooled
  4. extractionextracted with EtOAc (3×30 mL)
  5. washwashed with H2O, aq saturated NaHCO3 solution, brine
  6. dry with materialdried (Na2SO4)
  7. filtrationFiltration and concentration to dryness

出典と根拠

ORDレコード
ord-070f5b911b604575881b4138dfcb6ac2
出典データセット
uspto-grants-2001_10
特許番号
US06297239B1

関連ノート

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