Methanol → 3,7-Bis(2',2'-diphenylvinyl)-10-p-tolylphenothiazine

HRID 2287297노트

반응식

HRID 2287297 반응식
[CH:1]([C:3]1[CH:4]=[CH:5][C:6]2[N:7]([C:19]3[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][CH:20]=3)[C:8]3[C:13]([S:14][C:15]=2[CH:16]=1)=[CH:12][C:11]([CH:17]=O)=[CH:10][CH:9]=3)=O.[C:26]1([CH:32](P(=O)(OCC)OCC)[C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1.[CH3:47][C:48]([CH3:51])([O-])[CH3:49].[K+].CO>CN(C=O)C>[C:33]1([C:32]([C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=2)=[CH:1][C:3]2[CH:4]=[CH:5][C:6]3[N:7]([C:19]4[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][CH:20]=4)[C:8]4[C:13]([S:14][C:15]=3[CH:16]=2)=[CH:12][C:11]([CH:17]=[C:47]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:15][CH:16]=2)[C:48]2[CH:51]=[CH:13][CH:8]=[CH:9][CH:49]=2)=[CH:10][CH:9]=4)[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=1

참가 물질

6

반응물 4

HCID 887MethanolHCID 10267017Diethyl benzhydrylphosphonateHCID 187044763,7-Diformyl-10-p-tolylphenothiazineHCID 23665647Potassium tert-butoxide

생성물 1

HCID 187044733,7-Bis(2',2'-diphenylvinyl)-10-p-tolylphenothiazine수율 79%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In 20 ml of DMF were dissolved 2.0 g (5.8 mmol) of 3,7-diformyl-10-p-tolylphenothiazine (2b) and 4.0 g (13.2 mmol) of diethyl diphenylmethylphosphonate (3a). Thereto was gradually added 1.5 g (13.4 mmol) of potassium t-butoxide. After the mixture was reacted overnight, 10 ml of methanol was added thereto. The crystals precipitated were taken out by filtration, dissolved in chloroform, purified by silica gel column chromatography (toluene), and then recrystallized from a chloroform/hexane mixed solvent to obtain 1.48 g of the target compound.

후처리

  1. customAfter the mixture was reacted overnight
  2. customThe crystals precipitated
  3. filtrationwere taken out by filtration
  4. dissolutiondissolved in chloroform
  5. custompurified by silica gel column chromatography (toluene)
  6. customrecrystallized from a chloroform/hexane mixed solvent

출처 및 근거

ORD 기록
ord-8ef1f08c26b04b1f875d9eac75c9cfcf
출처 데이터셋
uspto-grants-2000_07
특허 번호
US06083651

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