4-Toluenesulfonyl chloride → HCID 53810576、化合物

HRID 65573ノート

反応式

HRID 65573 の反応式
[NH2:1][CH:2]([CH2:10][C:11]1[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=1)[C:3]([CH3:9])([CH3:8])[C:4]([O:6][CH3:7])=[O:5].C(N(CC)CC)C.[C:26]1([CH3:36])[CH:31]=[CH:30][C:29]([S:32](Cl)(=[O:34])=[O:33])=[CH:28][CH:27]=1>C(Cl)(Cl)Cl>[CH3:9][C:3]([CH3:8])([CH:2]([NH:1][S:32]([C:29]1[CH:30]=[CH:31][C:26]([CH3:36])=[CH:27][CH:28]=1)(=[O:34])=[O:33])[CH2:10][C:11]1[CH:12]=[CH:13][C:14]([O:17][CH3:18])=[CH:15][CH:16]=1)[C:4]([O:6][CH3:7])=[O:5]

参加物

5

反応物 3

HCID 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 23460866HCID 23460866、化合物

生成物 1

HCID 53810576HCID 53810576、化合物収率 85%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a solution of 251 g of methyl 3-amino-2,2-dimethyl-4-(p-methoxyphenyl)butyrate and 121 g of triethylamine in 750 ml of chloroform, there is added, with mechanical stirring and cooling with ice water, a solution of 210 g of p-toluenesulphonyl chloride in 500 ml of chloroform. After completion of the addition, which is carried out at such a rate that the temperature of the reaction mixture does not exceed 25° C., stirring is continued for 1.5 hours. Then the solution is washed with water, dilute hydrochloric acid and again with water, subsequently. After drying, the organic solvent is stripped off in vacuo. The residue is treated with ether, resulting in the crystallization of the title compound.

後処理

  1. additionAfter completion of the addition, which
  2. customdoes not exceed 25° C.
  3. stirringstirring
  4. washThen the solution is washed with water, dilute hydrochloric acid and again with water
  5. customAfter drying
  6. additionThe residue is treated with ether

出典と根拠

ORDレコード
ord-06e4ec385d9f4c278b56abdc9738a00b
出典データセット
uspto-grants-1978_12
特許番号
US04128548

反応ノート

読み込み中…