Dimethylformamide → HCID 58182722, 화합물

HRID 2191547노트

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HRID 2191547 반응식
[Br:1][C:2]1[N:6]=[C:5](Cl)[S:4][N:3]=1.[NH:8]1[CH2:13][CH2:12][CH:11]([NH:14][C:15](=[O:21])[O:16][CH2:17][CH:18]([CH3:20])[CH3:19])[CH2:10][CH2:9]1.CN(C=O)C>O>[Br:1][C:2]1[N:6]=[C:5]([N:8]2[CH2:9][CH2:10][CH:11]([NH:14][C:15](=[O:21])[O:16][CH2:17][CH:18]([CH3:19])[CH3:20])[CH2:12][CH2:13]2)[S:4][N:3]=1

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 27250533-Bromo-5-chloro-1,2,4-thiadiazoleHCID 15676964Isobutyl piperidin-4-ylcarbamate

생성물 1

HCID 58182722HCID 58182722, 화합물

시약·촉매·용매 1

HCID 962Water용매

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온도
100 °C

실험 절차

A mixture of 3-bromo-5-chloro-1,2,4-thiadiazole (0.21 g, 1.1 mmol), isobutyl piperidin-4-ylcarbamate (0.23 g, 1.2 mmol), and DMF (2 mL) was sealed in a microwave vessel and heated by microwave irradiation at 100° C. for two minutes. The reaction was cooled to room temperature, diluted with water, and extracted with CH2Cl2. The combined extracts were washed with water, dried over Na2SO4, and concentrated under reduced pressure to yield isobutyl 1-(3-bromo-1,2,4-thiadiazol-5-yl)piperidin-4-ylcarbamate. LC/MS: m/z 365.0 (M+H)+ at 3.20 min (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA)).

후처리

  1. customwas sealed in a microwave vessel
  2. temperatureThe reaction was cooled to room temperature
  3. extractionextracted with CH2Cl2
  4. washThe combined extracts were washed with water
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-9530f545dde54a1b883ee0468a89a5df
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08329702B2

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