Sulfuric Acid → Ethanol, 2-[2-(10H-phenothiazin-10-yl)ethoxy]-

HRID 2226739ノート

反応式

HRID 2226739 の反応式
O1CCCCC1[O:7][CH2:8][CH2:9][O:10][CH2:11][CH2:12][N:13]1[C:26]2[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=2[S:20][C:19]2[C:14]1=[CH:15][CH:16]=[CH:17][CH:18]=2.CC(O)C.S(=O)(=O)(O)O.[OH-].[Na+]>O>[CH:25]1[C:26]2[N:13]([CH2:12][CH2:11][O:10][CH2:9][CH2:8][OH:7])[C:14]3[C:19](=[CH:18][CH:17]=[CH:16][CH:15]=3)[S:20][C:21]=2[CH:22]=[CH:23][CH:24]=1

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 3776IsopropanolHCID 14798Sodium HydroxideHCID 18965314HCID 18965314、化合物

生成物 1

HCID 11822299Ethanol, 2-[2-(10H-phenothiazin-10-yl)ethoxy]-収率 52.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of crude 10-(2-(2-((tetrahydro-2-pyranyl)oxy)ethoxy)ethyl)-10H-phenothiazine (3.8 g, 10 mmol), 2-propanol (50 ml) and a 4 M aqueous sulfuric acid solution (8 ml) was heated at 60° C. for 3 h and then left overnight at room temperature. The reaction mixture was poured into a mixture of water (500 ml) and a 4 N sodium hydroxide solution (17 ml). The mixture was extracted with diethyl ether (150 ml) and the organic extract was washed with brine and dried over sodium sulphate. The solvent was evaporated in vacuo to give 1.5 g of crude 2-(2-(10H-phenothiazin-10-yl)ethoxy)ethanol. TLC: rf=0.52 (SiO2 ; dichloromethane/methanol=19:1).

後処理

  1. extractionThe mixture was extracted with diethyl ether (150 ml)
  2. extractionthe organic extract
  3. washwas washed with brine
  4. dry with materialdried over sodium sulphate
  5. customThe solvent was evaporated in vacuo

出典と根拠

ORDレコード
ord-3887336a9a3f46b2a6c294d7d686288f
出典データセット
uspto-grants-1994_09
特許番号
US05348965

反応ノート

読み込み中…