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Methyl iodide → HCID 178503951, 화합물

HRID 1054985
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HRID 1054985 반응식
[CH3:1][C:2]([CH3:15])=[CH:3][C:4]([NH:6][C:7]([N:9]1[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1)=[S:8])=[O:5].[C:16](=O)([O-])[O-].[Na+].[Na+].IC>O1CCCC1>[CH3:16][S:8]/[C:7](=[N:6]\[C:4](=[O:5])[CH:3]=[C:2]([CH3:15])[CH3:1])/[N:9]1[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1
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참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 10340Sodium CarbonateHCID 900174853-methyl-N-(piperidine-1-carbonothioyl)but-2-enamide

생성물 1

HCID 178503951HCID 178503951, 화합물수율 151%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 3-methyl-N-(piperidine-1-carbonothioyl)but-2-enamide (3.21 g, 14.2 mmol, Eq: 1.00), sodium carbonate (1.58 g, 14.9 mmol, Eq: 1.05) and iodomethane (10.1 g, 4.43 ml, 70.9 mmol, Eq: 5) in tetrahydrofuran (100 ml) was stirred for 2.5 days under reflux. The mixture was evaporated, 30 ml of ethyl acetate was added and the mixture was filtrated, the filtrate was evaporated affording 3-methyl-but-2-enoic acid 1-methylsulfanyl-1-piperidin-1-yl-meth-(Z)-ylideneamide (5.137 g, 151%) as an orange-brown semi-solid. MS: m/z=241.2 (M+H+)

후처리

  1. temperatureunder reflux
  2. customThe mixture was evaporated
  3. addition30 ml of ethyl acetate was added
  4. filtrationthe mixture was filtrated
  5. customthe filtrate was evaporated

출처 및 근거

ORD 기록
ord-8c5aa53044454fd592de83080465e964
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09394311B2

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