Hydrochloric Acid → N-(4-vinylbenzoyl)-4-methoxybenzenesulfonamide

HRID 363281

반응식

HRID 363281 반응식
Br[CH2:2][CH2:3][C:4]1[CH:23]=[CH:22][C:7]([C:8]([NH:10][S:11]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)(=[O:13])=[O:12])=[O:9])=[CH:6][CH:5]=1.N12CCCN=C1CCCCC2.Cl>C1COCC1>[CH:3]([C:4]1[CH:23]=[CH:22][C:7]([C:8]([NH:10][S:11]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)(=[O:13])=[O:12])=[O:9])=[CH:6][CH:5]=1)=[CH2:2]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 67587147N-[4-(2-bromoethyl)benzoyl]-4-methoxybenzenesulfonamide

생성물 1

HCID 15404407N-(4-vinylbenzoyl)-4-methoxybenzenesulfonamide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 35.85 g (0.09 mol) of N-[4-(2-bromoethyl)benzoyl]-4-methoxybenzenesulfonamide, 27.40 g (0.18 mol) of 1,8-diazabicyclo-[5.4.0]undec-7-ene (DBU) and 375 ml of THF was stirred at room temperature for 19.5 hrs. Solid formed within 30 mins. The mixture was poured into dilute HCl giving an oily precipitate which crystallized. The solid was collected, washed with water, redissolved in methylene chloride, dried over magnesium sulfate and concentrated to an oil which crystallized. The solid was collected, recrystallized from toluene, collected, washed with ligroine and dried.

후처리

  1. customSolid formed within 30 mins
  2. customcrystallized
  3. customThe solid was collected
  4. washwashed with water
  5. dissolutionredissolved in methylene chloride
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated to an oil which
  8. customcrystallized
  9. customThe solid was collected
  10. customrecrystallized from toluene
  11. customcollected
  12. washwashed with ligroine
  13. customdried

출처 및 근거

ORD 기록
ord-cbd759d9c45c482fbeab048a3d68cc39
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05874194

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