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Methyl iodide → 4-hydroxy-2-methyl-N-(2-thiazolyl)-2H-naphtho [2,1-e]-1,2-thiazine-3-carboxamide-1,1-dioxide

HRID 1730571
ノート
印刷プレビュー

反応式

HRID 1730571 の反応式
[OH-].[Na+].[OH:3][C:4]1[C:9]2[CH:10]=[CH:11][C:12]3[C:17]([C:8]=2[S:7](=[O:19])(=[O:18])[NH:6][C:5]=1[C:20]([NH:22][C:23]1[S:24][CH:25]=[CH:26][N:27]=1)=[O:21])=[CH:16][CH:15]=[CH:14][CH:13]=3.[CH3:28]I>CO>[OH:3][C:4]1[C:9]2[CH:10]=[CH:11][C:12]3[C:17]([C:8]=2[S:7](=[O:19])(=[O:18])[N:6]([CH3:28])[C:5]=1[C:20]([NH:22][C:23]1[S:24][CH:25]=[CH:26][N:27]=1)=[O:21])=[CH:16][CH:15]=[CH:14][CH:13]=3
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 546959454-Hydroxy-N-(2-thiazolyl)-2H-naphtho-[2,1-e]-1,2-thiazine-3-carboxamide-1,1-dioxide

生成物 1

HCID 547184104-hydroxy-2-methyl-N-(2-thiazolyl)-2H-naphtho [2,1-e]-1,2-thiazine-3-carboxamide-1,1-dioxide収率 40.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3.15 ml of 1 N sodium hydroxide (3.15 millimols) were added dropwise to a suspension of 1.12 gm (3 millimols) of 4-hydroxy-N-(2-thiazolyl) 2H-naphtho[2,1-e]-1,2-thiazine-3-carboxamide-1,1-dioxide in 50 ml of methanol and 1.7 gm (12 millimols) of methyl iodide, whereby a reddish solution was formed. The solution was stirred at room temperature for 72 hours and was then evaporated to dryness in vacuo. The residue was triturated with water, filterd off and recrystallized from ethylene chloride, yielding 0.47 gm (40.5% of theory) of 4-hydroxy-2-methyl-N-(2-thiazolyl)-2H-naphtho[2,1-e]-1,2-thiazine-3-carboxamide-1,1-dioxide, m.p. 249°-250° C (decomp).

後処理

  1. customwas formed
  2. customwas then evaporated to dryness in vacuo
  3. customThe residue was triturated with water, filterd off and
  4. customrecrystallized from ethylene chloride

出典と根拠

ORDレコード
ord-1909ea5b44df4dc9b74c1a31c41b4cc1
出典データセット
uspto-grants-1976_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03992535

反応ノート

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