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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Chloroacetic Acid → Acetic acid, [(5,7-dimethyl[1,2,4]triazolo[1,5-a]pyrimidin-2-yl)thio]-

HRID 1752788
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HRID 1752788 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]2[N:9]=[C:10]([SH:12])[N:11]=[C:4]2[N:3]=1.[OH-].[Na+].Cl[CH2:16][C:17]([OH:19])=[O:18].Cl>O>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]2[N:9]=[C:10]([S:12][CH2:16][C:17]([OH:19])=[O:18])[N:11]=[C:4]2[N:3]=1
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참가 물질

6

반응물 4

HCID 300Chloroacetic AcidHCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 178426287HCID 178426287, 화합물

생성물 1

HCID 714428Acetic acid, [(5,7-dimethyl[1,2,4]triazolo[1,5-a]pyrimidin-2-yl)thio]-

시약·촉매·용매 1

HCID 962Water용매

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온도
120 °C

실험 절차

A mixture of 5,7-Dimethyl-[1,2,4]triazolo[1,5-a]pyrimidine-2-thiol (1.0 g, 5.6 mmol), sodium hydroxide (0.44 g, 11.1 mmol), and water (22 mL) was added to a 100 mL RBF with a magnetic stirring bar. The flask was fitted with a condenser, and the mixture was warmed to reflux in a 120° C. oil bath for 30 min. The mixture was removed from the oil bath and allowed to cool, and chloroacetic acid (0.525 g, 5.6 mmol) was added. Warming to reflux was continued for 6 h. The mixture was allowed to cool to ambient temperature, and the pH was adjusted to 2 with 1 M aqueous hydrochloric acid (5 mL). A solid precipitate was isolated by filtration, rinsed with 1 M hydrochloric acid (2 mL) and water (5 mL), and allowed to dry. The title compound was obtained as a tan solid (1.16 g, 88% yield). 1H NMR (DMSO-d6, 400 MHz) δ ppm: 12.85 (br s, 1H), 7.12 (s, 1H), 4.08 (s, 2H), 2.66 (s, 3H), 2.54 (s, 3H).

후처리

  1. additionwas added to a 100 mL RBF with a magnetic stirring bar
  2. customThe flask was fitted with a condenser
  3. temperaturethe mixture was warmed
  4. customThe mixture was removed from the oil bath
  5. temperatureto cool
  6. temperatureWarming
  7. temperatureto reflux
  8. temperatureto cool to ambient temperature
  9. customA solid precipitate was isolated by filtration
  10. washrinsed with 1 M hydrochloric acid (2 mL) and water (5 mL)
  11. customto dry

출처 및 근거

ORD 기록
ord-01cd3b90424b419aa2e19a397d3e54cc
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09163027B2

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