Water → Thioxanthene

HRID 581647

반응식

HRID 581647 반응식
[CH:1]1[C:14]2[C:13](=O)[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[S:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3].CCOCC.O>C1C=CC=CC=1>[CH:1]1[C:14]2[CH2:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[S:6][C:5]=2[CH:4]=[CH:3][CH:2]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 3283Diethyl EtherHCID 10295ThioxanthoneHCID 21226445Aluminium lithium hydride

생성물 1

HCID 67495Thioxanthene수율 98%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A solution of thioxanthone (10 g) in 60 mL of benzene was treated with 5.0 g of LAH by stirring for 15 min. The mixture was heated and 100 mL of ether was added carefully. Reflux was continued for 90 min. The cooled mixture was neutralized with water. The solids were filtered off and the filtrate evaporated to dryness. Pure thioxanthene (9.1 g, 98%) was isolated by chromatography using 20% ethyl acetate/hexane; 1H NMR (CDCl3) δ 3.82 (s, 3H), 7.21 (m, 4H), 7.33 (m, 2H), 7.46 (m, 2H).

후처리

  1. temperatureThe mixture was heated
  2. temperatureReflux
  3. waitwas continued for 90 min
  4. filtrationThe solids were filtered off
  5. customthe filtrate evaporated to dryness

출처 및 근거

ORD 기록
ord-4a728b20ca324bcdb9d8d56c9eb6c534
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05922558

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