1,4-Dichlorobutane → HCID 11665882, 화합물

HRID 253687

반응식

HRID 253687 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 11665882HCID 11665882, 화합물

시약·촉매·용매 1

HCID 74236Tetrabutylammonium Bromide촉매

반응 조건

온도
95 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-1fb0f1f6a264471896e071da46f411ec
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07872132B2

연결된 노트

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