반응 #11320

반응 방정식

Thionyl chloride

1-methyl-D-tryptophan

MeOH

→

Intermediate 1

1-Methyl-D-tryptophan methyl ester hydrochloride

반응 조건

후처리

1. 1
   기타The solvent was removed under reduced pressure
2. 2
   기타triturated with Et2O (20 mL)
3. 3
   여과The solids were collected by vacuum filtration
4. 4
   기타dried in a vacuum oven at 60° C. for 3 days

실험 절차

Thionyl chloride (1.3 mL, 18.4 mmol) was added dropwise to a suspension of 1-methyl-D-tryptophan (2.0 g, 9.2 mmol) in MeOH (30 mL) at 0° C. under a nitrogen blanket. The resulting mixture was warmed slowly to room temperature and stirred for a total of 20 hours. The solvent was removed under reduced pressure and triturated with Et2O (20 mL). The solids were collected by vacuum filtration, then dried in a vacuum oven at 60° C. for 3 days to provide Intermediate 1 as an off-white powder, which was used without further purification (2.4 g, 96%): TLC Rf (1:2 EtOAc/CHCl3)=0.22.

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