Bromine → 2-Bromo-8-chloro-5-[(4-methoxyphenyl)sulfonyl]-6-methyl-5,6-dihydrophenanthridine

HRID 2181883ノート

反応式

HRID 2181883 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:13](=[CH:14][CH:15]=1)[C:12]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[N:6]([S:16]([C:19]1[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=1)(=[O:18])=[O:17])[CH:5]2[CH3:27].[Br:28]Br>C(O)(=O)C>[Br:28][C:10]1[CH:9]=[CH:8][C:7]2[N:6]([S:16]([C:19]3[CH:20]=[CH:21][C:22]([O:25][CH3:26])=[CH:23][CH:24]=3)(=[O:18])=[O:17])[CH:5]([CH3:27])[C:4]3[C:13](=[CH:14][CH:15]=[C:2]([Cl:1])[CH:3]=3)[C:12]=2[CH:11]=1

参加物

4

反応物 2

HCID 24408BromineHCID 22482264HCID 22482264、化合物

生成物 1

HCID 224823272-Bromo-8-chloro-5-[(4-methoxyphenyl)sulfonyl]-6-methyl-5,6-dihydrophenanthridine収率 61.3%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

The title compound was prepared from 8-chloro-5-[(4-methoxyphenyl)sulfonyl]-6-methyl-5,6-dihydrophenanthridine (0.95 g, 2.38 mmol), bromine (0.12 mL, 9.50 mmol), and glacial acetic acid (24 mL) according to the procedure and in the same manner as described in Example 4, step a. The crude product was purified by flash column chromatography on silica gel, eluting with a mixture of ethyl acetate-hexane (1:3 to 1:1 gradient) to yield 2-bromo-8-chloro-5-[(4-methoxyphenyl)sulfonyl]-6-methyl-5,6-dihydrophenanthridine (0.70 g, 1.46 mmol, 61%) as a white solid;

後処理

  1. customThe crude product was purified by flash column chromatography on silica gel
  2. washeluting with a mixture of ethyl acetate-hexane (1:3 to 1:1 gradient)

出典と根拠

ORDレコード
ord-0af10b7054634edea15ca83ab096a2de
出典データセット
uspto-grants-2005_05
特許番号
US06894061B2

反応ノート

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