Water → Thioxanthene

HRID 581647

反応式

HRID 581647 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 67495Thioxanthene収率 98%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-4a728b20ca324bcdb9d8d56c9eb6c534
出典データセット
uspto-grants-1999_07
特許番号
US05922558

関連ノート

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