Triphosgene → 8-Methoxy-1H-benzo[d][1,3]oxazine-2,4-dione

HRID 617127ノート

反応式

HRID 617127 の反応式
[NH2:1][C:2]1[C:10]([O:11][CH3:12])=[CH:9][CH:8]=[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>[CH3:12][O:11][C:10]1[C:2]2[NH:1][C:14]([O:5][C:4](=[O:6])[C:3]=2[CH:7]=[CH:8][CH:9]=1)=[O:16]

参加物

4

反応物 2

HCID 94429TriphosgeneHCID 2557202-Amino-3-methoxybenzoic acid

生成物 1

HCID 105596798-Methoxy-1H-benzo[d][1,3]oxazine-2,4-dione

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a chilled (0-5° C.) solution of 30.0 g (0.180 mol) of 2-amino-3-methoxybenzoic acid (Aldrich Chemicals) in 500 mL of tetrahydrofuran was added 17.8 g (0.0600 mol) of triphosgene. A precipitate formed upon addition. The ice bath was removed after 15 minutes, and the reaction mixture was stirred for 1 hour at room temperature. The reaction mixture was poured into 1000 mL of water and stirred for thirty minutes. The product (mp 267-268° C.) was filtered and amounted to 32.9 g.

後処理

  1. customA precipitate formed upon addition
  2. customThe ice bath was removed after 15 minutes
  3. additionThe reaction mixture was poured into 1000 mL of water
  4. stirringstirred for thirty minutes
  5. filtrationThe product (mp 267-268° C.) was filtered

出典と根拠

ORDレコード
ord-61941d03209842d88305795814a28779
出典データセット
uspto-grants-1999_09
特許番号
US05948775

反応ノート

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