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

HRID 2226739노트

반응식

HRID 2226739 반응식
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

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 3776IsopropanolHCID 14798Sodium HydroxideHCID 18965314HCID 18965314, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-3887336a9a3f46b2a6c294d7d686288f
출처 데이터셋
uspto-grants-1994_09
특허 번호
US05348965

반응 노트

불러오는 중…