Triphosgene → HCID 63109414、化合物

HRID 1688048ノート

反応式

HRID 1688048 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 63109414HCID 63109414、化合物収率 94%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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 H20. 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.

後処理

  1. additionadded
  2. concentrationThe reaction mixture was concentrated
  3. customthe resulting residue was sonicated in H20
  4. filtrationThe peach ppt was filtered
  5. concentrationwas concentrated under reduced pressure
  6. customIt was then azeotroped in toluene

出典と根拠

ORDレコード
ord-422dacc466cc4187b9af9336079a037f
出典データセット
uspto-grants-2012_04
特許番号
US08148391B2

反応ノート

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