Acetic Acid → 5-Hydroxy-12H-benzo[a]phenothiazine-7,7-dioxide

HRID 2352229ノート

反応式

HRID 2352229 の反応式
C([O:4][C:5]1[CH:18]=[C:17]2[C:8]([NH:9][C:10]3[C:15]([S:16]2(=[O:20])=[O:19])=[CH:14][CH:13]=[CH:12][CH:11]=3)=[C:7]2[CH:21]=[CH:22][CH:23]=[CH:24][C:6]=12)(=O)C.[OH-].[Na+].C(O)(=O)C>CO>[OH:4][C:5]1[CH:18]=[C:17]2[C:8]([NH:9][C:10]3[C:15]([S:16]2(=[O:20])=[O:19])=[CH:14][CH:13]=[CH:12][CH:11]=3)=[C:7]2[CH:21]=[CH:22][CH:23]=[CH:24][C:6]=12

参加物

5

反応物 3

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 13712482HCID 13712482、化合物

生成物 1

HCID 137124805-Hydroxy-12H-benzo[a]phenothiazine-7,7-dioxide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a suspension of 5-acetoxy-12H-benzo[a]phenothiazine-7,7-dioxide (6.6 g) in methanol (200 ml) there was added 2N aqueous sodium hydroxide solution (132 ml) and the mixture was stirred in the absence of air at room temperature for 7 minutes; at that point an amber solution had resulted. There was rapidly added 10% aqueous acetic acid solution (200 ml) causing precipitation of the title compound which was collected by filtration (5.68 g). A sample (500 mg) was crystallized from THF affording purified product (250 mg), m.p. 334° C. (dec).

後処理

  1. customat that point an amber solution had resulted
  2. customprecipitation of the title compound which
  3. filtrationwas collected by filtration (5.68 g)
  4. customA sample (500 mg) was crystallized from THF affording
  5. custompurified product (250 mg), m.p. 334° C. (dec)

出典と根拠

ORDレコード
ord-fba03f7a55de42a5bbed2d56313407d4
出典データセット
uspto-grants-1989_10
特許番号
US04876246

反応ノート

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