Hydrochloric Acid → 1-(9H-xanthen-2-yl)ethanone

HRID 65212

반응식

HRID 65212 반응식
[C:1](Cl)(=[O:3])[CH3:2].[Cl-].[Al+3].[Cl-].[Cl-].[CH:9]1[C:22]2[CH2:21][C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[O:14][C:13]=2[CH:12]=[CH:11][CH:10]=1.Cl>ClCCCl>[CH:9]1[C:22]2[CH2:21][C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[O:14][C:13]=2[CH:12]=[CH:11][C:10]=1[C:1]([CH3:2])=[O:3]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 7107XantheneHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 5151781-(9H-xanthen-2-yl)ethanone

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매3회

반응 조건

온도
16 °C

실험 절차

A 21.4 ml portion of acetyl chloride in 30 ml of 1,2-dichloroethane was added dropwise to 40 g of aluminum chloride in 105 ml of 1,2-dichloroethane. This mixture was stirred 1/2 hour and then added portionwise to an ice-cooled solution of 54.66 g of xanthene in 225 ml of 1,2-dichloroethane. The reaction was then allowed to warm to 16° C. and poured onto ice. A 180 ml portion of concentrated hydrochloric acid was added, the mixture was allowed to stand overnight and the layers separated. The aqueous layer was extracted with two 100 ml portions of chloroform then the organic layers was combined, dried, filtered through hydrous magnesium silicate and evaporated, giving the desired intermediate as a white crystalline solid, mp 103°-104° C.

후처리

  1. additionpoured onto ice
  2. waitto stand overnight
  3. customthe layers separated
  4. extractionThe aqueous layer was extracted with two 100 ml portions of chloroform
  5. customdried
  6. filtrationfiltered through hydrous magnesium silicate
  7. customevaporated

출처 및 근거

ORD 기록
ord-34713538c47747c8aa1843aa62c6c141
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04613611

연결된 노트

불러오는 중…