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

HRID 964949노트

반응식

HRID 964949 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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,

출처 및 근거

ORD 기록
ord-3e4168aafcfa4e9dbf0e366ed05a5c5b
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05773437

반응 노트

불러오는 중…