반응 #156665

반응 방정식

trimethylaluminum

4-(1,4-dioxa-7-aza-spiro[4.4]non-7-yl)-3-fluorophenylamine

6-methoxy-isochroman-1-one

Rochelle salt

→

N-[4-(1,4-Dioxa-7-aza-spiro[4.4]non-7-yl)-3-fluorophenyl]-2-(2-hydroxyethyl)-4-methoxy-benzamide

용매

toluene

methylene chloride

methylene chloride

반응 조건

후처리

1. 1
   workup.WAITfor 30 min at room temperature
2. 2
   workup.STIRRINGThe reaction mixture was stirred overnight at room temperature
3. 3
   workup.STIRRINGthe mixture was stirred for 1 h at room temperature
4. 4
   추출The aqueous phase was extracted several times with methylene chloride
5. 5
   건조dried over sodium sulfate
6. 6
   기타the solvent was removed in vacuum
7. 7
   기타In this way the product was obtained with molecular weight 416.17 (C22H25FN2O5)

실험 절차

A 2M solution of trimethylaluminum in toluene (14.9 mL) was added dropwise at 0° C. to a solution of 4-(1,4-dioxa-7-aza-spiro[4.4]non-7-yl)-3-fluorophenylamine (5.3 g) in methylene chloride (100.8 mL). The reaction mixture was stirred for 15 min at 0° C. and then for 30 min at room temperature. Then a solution of 6-methoxy-isochroman-1-one (3.8 g) in methylene chloride (40 mL) was added dropwise. The reaction mixture was stirred overnight at room temperature. Then saturated Rochelle salt solution was carefully added and the mixture was stirred for 1 h at room temperature. The aqueous phase was extracted several times with methylene chloride. The organic phases were combined, dried over sodium sulfate and the solvent was removed in vacuum. In this way the product was obtained with molecular weight 416.17 (C22H25FN2O5); MS (ESI): 417 (M+H+).

출처