Acetic Acid → 5,7-dichloro-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione

HRID 3103

반응식

HRID 3103 반응식
[Cl:1][C:2]1[CH:10]=[C:9]([Cl:11])[CH:8]=[C:7]2[C:3]=1[C:4](=[O:13])[C:5](=[O:12])[NH:6]2.C(O)(=[O:16])C>C(OC(=O)C)(=O)C.O.[O-2].[O-2].[O-2].[Cr+6]>[Cl:1][C:2]1[C:3]2[C:4](=[O:13])[O:12][C:5](=[O:16])[NH:6][C:7]=2[CH:8]=[C:9]([Cl:11])[CH:10]=1

참가 물질

6

반응물 2

HCID 176Acetic AcidHCID 2519084,6-Dichloroisatin

생성물 1

HCID 123632155,7-dichloro-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione수율 72%

시약·촉매·용매 3

HCID 10219390chromium (VI) trioxide촉매2회HCID 962Water용매HCID 7918Acetic Anhydride용매

실험 절차

To a stirred solution of 4,6-dichloro-1H-indole-2,3-dione (5.00 g, 23.2 mM) in acetic acid (21 mL) and acetic anhydride (21 mL) at 80° C. was added in small portions chromium trioxide (4.12 g, 41.3 mM). The temperature of the reaction mixture was maintained between 80°-90° C. during the addition of the chromium trioxide. After the addition was complete, the reaction mixture was diluted with water (100 mL) and then filtered to separate the precipitated solids. The solids were washed thoroughly with water and then dried to obtain the title compound as a yellow solid (4.13 g, 72%); MS(CI): 232 (M+H).

후처리

  1. additionAfter the addition
  2. filtrationfiltered
  3. customto separate the precipitated solids
  4. washThe solids were washed thoroughly with water
  5. customdried

출처 및 근거

ORD 기록
ord-62f911c33ec34c2dbe633593e1d5ee82
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733910

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