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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Water → 6-Bromochromone-3-carboxylic acid

HRID 2058950
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HRID 2058950 반응식
[C:1]([C:3]1[C:12](=[O:13])[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([Br:14])[CH:10]=2)[O:5][CH:4]=1)#N.N([O-])=[O:16].[Na+].[OH2:19]>S(=O)(=O)(O)O>[Br:14][C:9]1[CH:10]=[C:11]2[C:6](=[CH:7][CH:8]=1)[O:19][CH:1]=[C:3]([C:4]([OH:16])=[O:5])[C:12]2=[O:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962Water2회HCID 7030366-Bromochromone-3-carbonitrileHCID 23668193Sodium Nitrite

생성물 1

HCID 27568986-Bromochromone-3-carboxylic acid

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

26 g of the product of step (b) are stirred overnight in 150 ml of conc. sulphuric acid at room temperature. The mixture is then diluted with 10 ml of water and cooled to 0°. Under stirring, a solution of 15 g of sodium nitrite in 30 ml of water is introduced slowly under the liquid surface, the temperature being maintained by cooling at 15°. After addition, the mixture is warmed at 70° for 1 hour and poured over ice and the precipitate is suction filtered off, suspended in 600 ml of acetone, refluxed, hot-filtered and the filtrate then evaporated on a rotary evaporator. The residue is recrystallised from chloroform, to obtain the heading compound, m.p. 260°-264°.

후처리

  1. temperaturecooled to 0°
  2. temperaturethe temperature being maintained
  3. temperatureby cooling at 15°
  4. additionAfter addition
  5. temperaturethe mixture is warmed at 70° for 1 hour
  6. additionpoured over ice
  7. filtrationfiltered off
  8. temperaturerefluxed
  9. filtrationhot-filtered
  10. customthe filtrate then evaporated on a rotary evaporator
  11. customThe residue is recrystallised from chloroform
  12. customto obtain the heading compound, m.p. 260°-264°

출처 및 근거

ORD 기록
ord-eeac1303aefb4dce8191dd94ffa4d5a7
출처 데이터셋
uspto-grants-1982_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04320133

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