Water → 5-Chloro-7-trifluoromethyl-2H-3,1-benzoxazine-2,4(1H)-dione

HRID 3130

반응식

HRID 3130 반응식
[NH2:1][C:2]1[CH:10]=[C:9]([Cl:11])[CH:8]=[C:7]([C:12]([F:15])([F:14])[F:13])[C:3]=1C(O)=O.ClC(O[C:21](=[O:27])[O:22][C:23](Cl)(Cl)Cl)(Cl)Cl.[OH2:28]>O1CCCC1>[Cl:11][C:9]1[C:10]2[C:23](=[O:28])[O:22][C:21](=[O:27])[NH:1][C:2]=2[CH:3]=[C:7]([C:12]([F:13])([F:14])[F:15])[CH:8]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 94429TriphosgeneHCID 189299122-Amino-4-chloro-6-trifluoromethylbenzoic acid

생성물 1

HCID 189299275-Chloro-7-trifluoromethyl-2H-3,1-benzoxazine-2,4(1H)-dione

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of 2-amino-4-chloro-6-trifluoromethylbenzoic acid (0.53 g, 2.2 mM) in dry tetrahydrofuran (6 mL) under a nitrogen atmosphere was added bis(trichloromethyl)carbonate (0.218 g, 0.734 mM). The resulting solution was stirred at room temperature for 2 hr, poured into water and the resulting mixture extracted with ethyl acetate. The combined extracts were dried (MgSO4), filtered and concentrated to leave the title compound as a tan solid; MS(CI): 266 (M+H).

후처리

  1. extractionthe resulting mixture extracted with ethyl acetate
  2. dry with materialThe combined extracts were dried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-0600c001c51645919f6df926c38c5514
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733910

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