Toluene → 5,6-dichloro-1H-indene
反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[Cl:11])[CH:7](O)[CH2:6][CH2:5]2.C1(C)C=CC=CC=1.C1(C)C=CC(S(O)(=O)=O)=CC=1.[OH-].[Na+]>O.C(C1C=C(O)C(=CC=1)O)(C)(C)C>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[Cl:11])[CH2:7][CH:6]=[CH:5]2参加物
7
実験手順
A mixture of 17.48 g of the product of Step B, 470 ml of toluene, 0.57 g of 4-tert.-butyl-catechol and 1.63 g of p-toluene sulfonic acid was refluxed for 2 hours and then was diluted with water. 10 ml of N sodium hydroxide solution were added and the mixture was extracted with toluene. The organic phase was evaporated to dryness under reduced pressure and the residue was taken up in hexane. The mixture was vacuum filtered and the crystalline product was dried to obtain 9 g of the desired product melting at 76° C.
後処理
- temperaturewas refluxed for 2 hours
- extractionthe mixture was extracted with toluene
- customThe organic phase was evaporated to dryness under reduced pressure
- filtrationfiltered
- customthe crystalline product was dried
出典と根拠
- ORDレコード
- ord-697626cccf67485283f663d344ef5127
- 出典データセット
- uspto-grants-1994_09
- 特許番号
- US05348971
反応ノート
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