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Water → HCID 25260863, 화합물

HRID 1966202
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HRID 1966202 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9]([NH2:11])=[S:10])=[N:6][CH:7]=1.[CH2:12]([O:14][C:15](=[O:20])[C:16](=O)[CH2:17]Br)[CH3:13].O>CN(C=O)C>[CH2:12]([O:14][C:15]([C:16]1[N:11]=[C:9]([NH:8][C:5]2[CH:4]=[CH:3][C:2]([Br:1])=[CH:7][N:6]=2)[S:10][CH:17]=1)=[O:20])[CH3:13]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 66144Ethyl bromopyruvateHCID 234388741-(5-Bromopyridin-2-yl)thiourea

생성물 1

HCID 25260863HCID 25260863, 화합물수율 78%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
70 °C

실험 절차

(5-Bromo-pyridine-2-yl)-thiourea (1 mmol) is dissolved in DMF (2 ml) and 3-Bromo-2-oxo-propionic acid ethyl ester (1 eq.) is added and stirred 2 h at 70° C. The suspension is diluted with DMF (2 ml). After cooling to RT the reaction solution is poured into water and the resulting precipitate is filtered, washed with water and dried 16 h in vacuo at 40° C. “A4” is obtained as colourless powder in a yield of 78%; mp. 299.8-300.8° C.; HPLC (method C): 2.01 min; LC-MS (method A): 2.002 min, 327.95 (M+H+);

후처리

  1. temperatureAfter cooling to RT the reaction solution
  2. filtrationthe resulting precipitate is filtered
  3. washwashed with water
  4. dry with materialdried 16 h in vacuo at 40° C. “A4”
  5. customis obtained as colourless powder in a yield of 78%
  6. custom2.01 min
  7. custom2.002 min, 327.95 (M+H+)

출처 및 근거

ORD 기록
ord-0892a73dd1bc414889ed1cac52d3d923
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08420642B2

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