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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Methyl iodide → 4-Bromo-2,3,7-trimethoxy-10H-phenothiazine

HRID 231058
ノート
印刷プレビュー

反応式

HRID 231058 の反応式
[Br:1][C:2]1[C:15]2[S:14][C:13]3[C:8](=[CH:9][CH:10]=[C:11]([O:16][CH3:17])[CH:12]=3)[NH:7][C:6]=2[CH:5]=[C:4]([O:18][CH3:19])[C:3]=1[OH:20].CI.[C:23](=O)([O-])[O-].[K+].[K+]>CN(C=O)C.O.C(OCC)(=O)C>[Br:1][C:2]1[C:15]2[S:14][C:13]3[C:8](=[CH:9][CH:10]=[C:11]([O:16][CH3:17])[CH:12]=3)[NH:7][C:6]=2[CH:5]=[C:4]([O:18][CH3:19])[C:3]=1[O:20][CH3:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium Carbonate2 回HCID 138537384-bromo-2,7-dimethoxy-3-hydroxy-10H-phenothiazine

生成物 1

HCID 138820384-Bromo-2,3,7-trimethoxy-10H-phenothiazine収率 36.7%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 4-bromo-2,7-dimethoxy-3-hydroxy-10H-phenothiazine (3.54 g) and methyliodide (2.5 ml) in DMF (20 ml) there was added pulverized potassium carbonate (1.3 g). The reaction mixture was stirred at room temperature. After 15 minutes, another addition of potassium carbonate (1 gram) was made, followed by two other such additions at 15-minute intervals. The final mixture was stirred for a further 15 minutes, then it was diluted with water (100 ml) and ethyl acetate (100 ml). The organic layer was washed twice with water, dried and evaporated down to a solid residue. Crystallization from acetone followed by column chromatography on silica gel eluting with 1:19 ethyl acetate-dichloromethane afforded the pure title compound (1.27 g). m.p. 223°-225° C.

後処理

  1. waitfollowed by two other such additions at 15-minute
  2. washThe organic layer was washed twice with water
  3. customdried
  4. customevaporated down to a solid residue
  5. customCrystallization from acetone

出典と根拠

ORDレコード
ord-bfe542a4bbf14ecbbad90eae15d95663
出典データセット
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04845083

反応ノート

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