Hydrochloric Acid → 2-(3-Chloropropyl)-2H-1,2-benzothiazin-4(3H)-one 1,1-Dioxide

HRID 964949ノート

反応式

HRID 964949 の反応式
C1O[C:4]2([C:9]3[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=3[S:7](=[O:15])(=[O:14])[N:6]([CH2:16][CH2:17][CH2:18][Cl:19])[CH2:5]2)[O:3]C1.Cl>CO>[Cl:19][CH2:18][CH2:17][CH2:16][N:6]1[CH2:5][C:4](=[O:3])[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[S:7]1(=[O:15])=[O:14]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 121117312-(3-Chloropropyl)-2H-1,2-benzothiazin-4(3H)-one 1,1-dioxide Ethylene Ketal

生成物 1

HCID 187599102-(3-Chloropropyl)-2H-1,2-benzothiazin-4(3H)-one 1,1-Dioxide収率 100%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 2-(3-chloropropyl)-2H-1,2-benzothiazin-4(3H)-one 1,1-dioxide ethylene ketal (5.0 g, 15.7 mmol.), 3N aqueous hydrochloric acid (30 mL) and methanol (30 mL) was heated under refluxing for 20 min. Methanol was distilled off under reduced pressure. To the residue was added water (30 mL), and the mixture was extracted with ethyl ether. The ethyl ether portion was washed with an aqueous saturated sodium chloride solution, dried over anhydrous sodium sulfate, and placed under reduced pressure to distill the solvent off, to give the desired compound (4.19 g, 100%) as a yellow oil.

後処理

  1. temperaturewas heated
  2. temperatureunder refluxing for 20 min
  3. distillationMethanol was distilled off under reduced pressure
  4. additionTo the residue was added water (30 mL)
  5. extractionthe mixture was extracted with ethyl ether
  6. washThe ethyl ether portion was washed with an aqueous saturated sodium chloride solution
  7. dry with materialdried over anhydrous sodium sulfate
  8. distillationto distill the solvent off,

出典と根拠

ORDレコード
ord-3e4168aafcfa4e9dbf0e366ed05a5c5b
出典データセット
uspto-grants-1998_06
特許番号
US05773437

反応ノート

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