Water → HCID 86723563, 화합물

HRID 2201657노트

반응식

HRID 2201657 반응식
[CH2:1]=[C:2]1[CH2:5][CH:4]([CH2:6][NH2:7])[CH2:3]1.C([O-])([O-])=O.[Na+].[Na+].Cl[C:15]([O:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[O:16].O>O1CCCC1>[CH2:1]=[C:2]1[CH2:5][CH:4]([CH2:6][NH:7][C:15](=[O:16])[O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH2:3]1

참가 물질

6

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 10387Benzyl chloroformateHCID 177500821-(3-Methylidenecyclobutyl)methanamine

생성물 1

HCID 86723563HCID 86723563, 화합물수율 56.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Compound 4-2 (3 g, 30.9 mmol) was dissolved in 50 mL of tetrahydrofuran, added Na2CO3 (6.3 g, 60 mmol) and benzyl chloroformate (5.25 g, 30.8 mmol). The mixture was stirred for 12 hours at room temperature, added 100 mL of water, extracted three times with 300 mL of ethyl acetate, combined the organic phases, rotary evaporated to remove solvents and purified by column chromatography (petroleum ether/ethyl acetate=10:1) to give Compound 4-3 (4 g, 56% yield).

후처리

  1. extractionextracted three times with 300 mL of ethyl acetate
  2. customrotary evaporated
  3. customto remove solvents
  4. custompurified by column chromatography (petroleum ether/ethyl acetate=10:1)

출처 및 근거

ORD 기록
ord-eef0e8133ab7412380e1dd79abf4ccb8
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09365499B2

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