Triethylamine → 7-chloro-9-methyl-5-(N-ethylsulfonylamino)-2,3,4,5-tetrahydro-1-benzoxepine

HRID 2271082ノート

反応式

HRID 2271082 の反応式
[CH2:1]([S:3](Cl)(=[O:5])=[O:4])[CH3:2].[NH2:7][CH:8]1[C:14]2[CH:15]=[C:16]([Cl:20])[CH:17]=[C:18]([CH3:19])[C:13]=2[O:12][CH2:11][CH2:10][CH2:9]1.C(N(CC)CC)C>C1COCC1>[Cl:20][C:16]1[CH:17]=[C:18]([CH3:19])[C:13]2[O:12][CH2:11][CH2:10][CH2:9][CH:8]([NH:7][S:3]([CH2:1][CH3:2])(=[O:5])=[O:4])[C:14]=2[CH:15]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 11667Ethanesulfonyl chlorideHCID 223917895-Amino-7-chloro-9-methyl-2,3,4,5-tetrahydro-1-benzoxepine

生成物 1

HCID 223917937-chloro-9-methyl-5-(N-ethylsulfonylamino)-2,3,4,5-tetrahydro-1-benzoxepine収率 85.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

0.86 g of ethanesulfonyl chloride was added dropwise with ice-cooling to a solution of 1.3 g of 5-amino-7-chloro-9-methyl-2,3,4,5-tetrahydro-1-benzoxepine and 2.4 g of triethylamine in 30 ml of THF. The mixture was allowed to come to room temperature and was stirred overnight, and the solvent was distilled off in vacuo. After stirring the residue with water, the deposited product was filtered off with suction and dried in vacuo. 1.6 g of 7-chloro-9-methyl-5-(N-ethylsulfonylamino)-2,3,4,5-tetrahydro-1-benzoxepine were obtained, m.p. 144-145° C.

後処理

  1. customto come to room temperature
  2. distillationthe solvent was distilled off in vacuo
  3. stirringAfter stirring the residue with water
  4. filtrationthe deposited product was filtered off with suction
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-2395683f46e5417698c5c6252117a9e5
出典データセット
uspto-grants-2001_12
特許番号
US06333349B1

反応ノート

読み込み中…