Butylurea → N-(4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]-benzenesulfonyl)-N'-butyl-urea

HRID 894095

反応式

HRID 894095 の反応式
[CH2:1]([NH:5][C:6]([NH2:8])=[O:7])[CH2:2][CH2:3][CH3:4].[H-].[Na+].[O:11]=[C:12]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH2:14][N:13]1[C:21]([NH:23][CH2:24][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:22].[S:32](Cl)(O)(=[O:34])=[O:33]>O1CCCC1>[O:11]=[C:12]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH2:14][N:13]1[C:21]([NH:23][CH2:24][CH2:25][C:26]1[CH:31]=[CH:30][C:29]([S:32]([NH:8][C:6]([NH:5][CH2:1][CH2:2][CH2:3][CH3:4])=[O:7])(=[O:34])=[O:33])=[CH:28][CH:27]=1)=[O:22]

参加物

5

反応物 3

HCID 11595ButylureaHCID 24758Sodium hydrideHCID 211623494-[2-(1-Oxo-isoindoline-2-carboxamido)-ethyl]-benzene sulfochloride

生成物 1

HCID 21162325N-(4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]-benzenesulfonyl)-N'-butyl-urea

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

4.8 g of butyl urea are dissolved in 100 ml of tetrahydrofurane and, while stirring, 1.5 g of 80% sodium hydride (in oil) are added. The mixture is heated for 3 hours to 60° C. whereupon 7.6 g of 4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]-benzene-sulfochloride in 100 ml of tetrahydrofurane are added while cooling. The temperature is slowly raised to 60°-70° C. and stirring is continued at that temperature for 3 hours. The solvent is removed under reduced pressure, water is added to the residue, the mixture is filtered and the filtrate is acidified with dilute hydrochloric acid. After recrystallization from dilute acetone, the N-(4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]benzenesulfonyl)-N'-butyl-urea melts at 189°-190° C.

後処理

  1. additionare added
  2. temperaturewhile cooling
  3. temperatureThe temperature is slowly raised to 60°-70° C.
  4. stirringstirring
  5. customThe solvent is removed under reduced pressure, water
  6. additionis added to the residue
  7. filtrationthe mixture is filtered
  8. customAfter recrystallization from dilute acetone

出典と根拠

ORDレコード
ord-eeaef196eedc4b268efebd985dfcd232
出典データセット
uspto-grants-1981_08
特許番号
US04282239

関連ノート

読み込み中…