Diethylamine → Benzo[b][1,4]thiazepin-4(5H)-one, 2,3-dihydro-3-acetoxy-2-(4-methoxyphenyl)-

HRID 1649328ノート

反応式

HRID 1649328 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH:15]([O:16][C:17](=[O:19])[CH3:18])[C:14](=[O:20])[N:13](C(=O)C)[C:12]3[CH:24]=[CH:25][CH:26]=[CH:27][C:11]=3[S:10]2)=[CH:5][CH:4]=1.C(NCC)C>C(Cl)(Cl)Cl>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH:9]2[CH:15]([O:16][C:17](=[O:19])[CH3:18])[C:14](=[O:20])[NH:13][C:12]3[CH:24]=[CH:25][CH:26]=[CH:27][C:11]=3[S:10]2)=[CH:7][CH:8]=1

参加物

4

反応物 2

HCID 8021DiethylamineHCID 132366692-(4'-Methoxyphenyl)-3-acetoxy-5-acetyl-2,3-dihydro-1,5-benzothiazepin-4(5H)-one2 回

生成物 1

HCID 591255Benzo[b][1,4]thiazepin-4(5H)-one, 2,3-dihydro-3-acetoxy-2-(4-methoxyphenyl)-収率 94.8%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

7-(1). 2-(4'-Methoxyphenyl)-3-acetoxy-5-acetyl-2,3-dihydro-1,5-benzothiazepin-4(5H)-one [Compound (VII)] (1.93 g) and diethylamine (0.44 g) are added to chloroform (20 ml), and the mixture is stirred at room temperature for one hour. After distilling off chloroform, water is added to the residue, and the precipitated crystals are separated by filtration, washed with water and dried to give the title compound (II) (1.63 g, 94.8%), m.p. 198°-200° C.

後処理

  1. distillationAfter distilling off chloroform, water
  2. additionis added to the residue
  3. customthe precipitated crystals are separated by filtration
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-55ea379747b34aa6b34df4dfe3a62e1b
出典データセット
uspto-grants-1983_11
特許番号
US04416819

反応ノート

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