Methyl iodide → HCID 21473342, 화합물

HRID 440248

반응식

HRID 440248 반응식
[H-].[Na+].[CH3:3]I.[C:5]([O:9][C:10]([N:12]1[CH2:16][CH:15]([NH:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:14]([OH:24])[CH2:13]1)=[O:11])([CH3:8])([CH3:7])[CH3:6]>O1CCCC1>[C:5]([O:9][C:10]([N:12]1[CH2:16][CH:15]([NH:17][C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)[CH:14]([O:24][CH3:3])[CH2:13]1)=[O:11])([CH3:8])([CH3:6])[CH3:7]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 214733471-t-Butoxycarbonyl-3-hydroxy-4-phenylaminopyrrolidine

생성물 1

HCID 21473342HCID 21473342, 화합물수율 79.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To 10 ml of anhydrous tetrahydrofuran was added 0.34 g (0.0085 mole) of a 60% sodium hydride-mineral oil, and while stirring the mixture at 45° to 50° C., 1.21 g (0.0085 mole) of methyl iodide was added thereto. To the mixture was added dropwise a solution of 2.37 g of 1-t-butoxycarbonyl-3-hydroxy-4-phenylaminopyrrolidine obtained in Reference example 17 (1) dissolved in 10 ml of anhydrous tetrahydrofuran, and the mixture was further stirred at the same temperature for 1 hour. After the mixture was cooled to room temperature, the solvent was removed under reduced pressure, and the residue was supplied to silica gel column chromatography (the eluent used was a mixture of methyl acetate: toluene = 1 : 4) to obtain 1.98 g of 1-t-butoxycarbonyl-3-methoxy-4-phenylaminopyrrolidine as white crystals.

후처리

  1. stirringthe mixture was further stirred at the same temperature for 1 hour
  2. customthe solvent was removed under reduced pressure
  3. additiona mixture of methyl acetate

출처 및 근거

ORD 기록
ord-96053ac08ae847158f1522d21ca752eb
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05519016

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