1,4-Dichlorobutane → HCID 11665882、化合物

HRID 253687

反応式

HRID 253687 の反応式
[OH:1][C:2]1[CH:10]=[C:9]2[C:5]([CH2:6][CH2:7][C:8]2=[O:11])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[Cl:18][CH2:19][CH2:20][CH2:21][CH2:22]Cl>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC>[Cl:18][CH2:19][CH2:20][CH2:21][CH2:22][O:1][C:2]1[CH:10]=[C:9]2[C:5]([CH2:6][CH2:7][C:8]2=[O:11])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 80591,4-DichlorobutaneHCID 11430Potassium CarbonateHCID 70206596-Hydroxy-1-indanone

生成物 1

HCID 11665882HCID 11665882、化合物

試薬・触媒・溶媒 1

HCID 74236Tetrabutylammonium Bromide触媒

反応条件

温度
95 °C

実験手順

Mixture of 6-hydroxyindan-1-one of the formula (11) (20 gm, 0.135 mol), potassium carbonate (40 gm, 0.289 mol), 1,4-dichlorobutane (80 ml, 0.73 mol) and tetrabutyl ammonium bromide (2 g) was stirred for 1-3 hrs at 95° C. then distilled off excess 1,4-dichloro butane, diluted with water (80 ml). The aqueous layer was extracted with ethyl acetate, and the extract was washed with water, dried and evaporated off under reduced pressure to dryness. The evaporation residue is purified by crystallization using isopropyl ether as a solvent gave 29.5 gm of novel 6-(4-CHLORO BUTOXY)-INDAN-1-ONE of the formula (3).

後処理

  1. distillationthen distilled off excess 1,4-dichloro butane
  2. additiondiluted with water (80 ml)
  3. extractionThe aqueous layer was extracted with ethyl acetate
  4. washthe extract was washed with water
  5. customdried
  6. customevaporated off under reduced pressure to dryness
  7. customThe evaporation residue is purified by crystallization

出典と根拠

ORDレコード
ord-1fb0f1f6a264471896e071da46f411ec
出典データセット
uspto-grants-2011_01
特許番号
US07872132B2

関連ノート

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