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

HRID 363281

反応式

HRID 363281 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cbd759d9c45c482fbeab048a3d68cc39
出典データセット
uspto-grants-1999_02
特許番号
US05874194

関連ノート

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