Salicylamide → 2,2-dimethyl-3,4-dihydro-2H-1,3-benzoxazin-4-one

HRID 259225

反応式

HRID 259225 の反応式
C(Cl)(Cl)Cl.[C:5]([NH2:14])(=[O:13])[C:6]1[C:7](=[CH:9][CH:10]=[CH:11][CH:12]=1)[OH:8].O.[C:16]1(C)[C:17](S(O)(=O)=O)=CC=C[CH:21]=1>CC(C)=O>[CH3:21][C:16]1([CH3:17])[NH:14][C:5](=[O:13])[C:6]2[CH:12]=[CH:11][CH:10]=[CH:9][C:7]=2[O:8]1

参加物

5

反応物 3

HCID 5147SalicylamideHCID 6212ChloroformHCID 124969952-Methylbenzenesulfonic acid hydrate

生成物 1

HCID 7174282,2-dimethyl-3,4-dihydro-2H-1,3-benzoxazin-4-one

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

A 500-ml flask was charged with 250 ml of chloroform, 27.4 g (0.2 mol) of salicylamide, 23.2 g (0.4 mol) of acetone and 2.7 g of toluene sulfonic acid monohydrate. The flask was equipped with a Soxhlet extraction vessel containing 36.7 g of molecular sieves (Linde Type 3A, 1/16 inch) in the thimble. The reaction mixture was refluxed for 24 hours. Then fresh sieves were placed in the Soxhlet and 10 g of acetone was added to the reaction mixture. Reflux was continued for 24 hours.

後処理

  1. customThe flask was equipped with a Soxhlet extraction vessel
  2. temperatureThe reaction mixture was refluxed for 24 hours
  3. additionwas added to the reaction mixture
  4. temperatureReflux

出典と根拠

ORDレコード
ord-b2ffb7e073fb4b8f88697099e8fecc7d
出典データセット
uspto-grants-1977_07
特許番号
US04036960

関連ノート

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