Triphosgene → HCID 63109414, 화합물

HRID 1041706노트

반응식

HRID 1041706 반응식
[NH2:1][C:2]1[C:10]([F:11])=[CH:9][C:8]([F:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].Cl[C:14](Cl)([O:16]C(=O)OC(Cl)(Cl)Cl)Cl>O1CCCC1>[F:12][C:8]1[CH:9]=[C:10]([F:11])[C:2]2[NH:1][C:14](=[O:16])[O:5][C:4](=[O:6])[C:3]=2[CH:7]=1

참가 물질

4

반응물 2

HCID 94429TriphosgeneHCID 146519732-Amino-3,5-difluorobenzoic acid

생성물 1

HCID 63109414HCID 63109414, 화합물수율 94%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

2-Amino-3,5-difluoro-benzoic acid (2.44 g, 0.0141 mol) was dissolved in Tetrahydrofuran (100 mL). Triphosgene (4.18 g, 0.0141 mol) was dissolved in Tetrahydrofuran (10 mL) and added. The resulting solution was stirred for 4 h at rt. The reaction mixture was concentrated, and the resulting residue was sonicated in H2O. The peach ppt was filtered, taken up in acetone, and was concentrated under reduced pressure. It was then azeotroped in toluene to give 6,8-Difluoro-1H-3,1-benzoxazine-2,4-dione as tan solids (2.64 g, 94%). 1H-NMR (DMSO): 12.00 (s, 1H), 7.85 (m, 1H), 7.60 (m, 1H); 19F-NMR (DMSO): −116, −125.

후처리

  1. additionadded
  2. concentrationThe reaction mixture was concentrated
  3. customthe resulting residue was sonicated in H2O
  4. filtrationThe peach ppt was filtered
  5. concentrationwas concentrated under reduced pressure
  6. customIt was then azeotroped in toluene

출처 및 근거

ORD 기록
ord-ad44d9fa2314443c9267ae138b8bd28a
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08552186B2

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