Nitrogen → 7-bromo-3-fluoro-2-methoxy-9H-xanthen-9-one

HRID 335917

반응식

HRID 335917 반응식
N#N.OS(O)(=O)=O.[Br:8][C:9]1[CH:27]=[CH:26][C:12]([O:13][C:14]2[CH:22]=[C:21]([F:23])[C:20]([O:24][CH3:25])=[CH:19][C:15]=2[C:16]([OH:18])=O)=[CH:11][CH:10]=1>>[Br:8][C:9]1[CH:10]=[C:11]2[C:12]([O:13][C:14]3[CH:22]=[C:21]([F:23])[C:20]([O:24][CH3:25])=[CH:19][C:15]=3[C:16]2=[O:18])=[CH:26][CH:27]=1

참가 물질

4

반응물 3

HCID 947NitrogenHCID 1118Sulfuric AcidHCID 67383032HCID 67383032, 화합물

생성물 1

HCID 584662337-bromo-3-fluoro-2-methoxy-9H-xanthen-9-one

반응 조건

온도
60 °C

실험 절차

A 3 neck 22 L RBF equipped with a mechanical stirrer, temperature probe and N2 inlet was charged with concentrated H2SO4 (2.7 L) and heated to 60° C. To this mixture was added 2-(4-bromophenoxy)-4-fluoro-5-methoxybenzoic acid (1.3 kg, 3.81 mol) in portions such that the internal temp remained below 70° C. The resulting mixture was stirred at 60° C. for 1 hour at which point the reaction mixture was cooled to 0° C. and slowly poured onto ice water. The resulting solids were removed by filtration, washed with water and triturated with EtOAc (3 L). The solid was then washed with EtOAc, hexane and dried under vacuum at 30° C. to afford 7-bromo-3-fluoro-2-methoxy-9H-xanthen-9-one as an off white solid.

후처리

  1. customA 3 neck 22 L RBF equipped with a mechanical stirrer
  2. customremained below 70° C
  3. temperaturewas cooled to 0° C.
  4. additionslowly poured onto ice water
  5. customThe resulting solids were removed by filtration
  6. washwashed with water
  7. customtriturated with EtOAc (3 L)
  8. washThe solid was then washed with EtOAc, hexane
  9. customdried under vacuum at 30° C.

출처 및 근거

ORD 기록
ord-cfb04d01f6fe43b281519cb09a1c7e68
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08883782B2

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