Hydrochloric Acid → 1,3-Bis[4-[(3,5-dioxo-1,2,4-oxadiazolidin-2-yl)methyl]phenoxy]benzene

HRID 263541노트

반응식

HRID 263541 반응식
[OH:1][NH:2][CH2:3][C:4]1[CH:26]=[CH:25][C:7]([O:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([O:15][C:16]3[CH:21]=[CH:20][C:19]([CH2:22][NH:23][OH:24])=[CH:18][CH:17]=3)[CH:10]=2)=[CH:6][CH:5]=1.C(O[C:32]([N:34]=[C:35]=[O:36])=[O:33])CCC.[OH-:37].[Na+].Cl>O1CCCC1>[O:37]=[C:35]1[NH:34][C:32](=[O:33])[O:24][N:23]1[CH2:22][C:19]1[CH:20]=[CH:21][C:16]([O:15][C:11]2[CH:12]=[CH:13][CH:14]=[C:9]([O:8][C:7]3[CH:25]=[CH:26][C:4]([CH2:3][N:2]4[C:35](=[O:36])[NH:34][C:32](=[O:33])[O:1]4)=[CH:5][CH:6]=3)[CH:10]=2)=[CH:17][CH:18]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 12538171Butyloxycarbonyl isocyanateHCID 190384471,3-Bis[4-(N-hydroxyaminomethyl)phenoxy]benzene

생성물 1

HCID 190384251,3-Bis[4-[(3,5-dioxo-1,2,4-oxadiazolidin-2-yl)methyl]phenoxy]benzene

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

1,3-bis[4-(N-hydroxyaminomethyl)phenoxy]benzene (1.76 g) was dissolved in 35 ml of tetrahydrofuran to which, with ice-cooling and in an atmosphere of argon, was subsequently added dropwise 1.65 g of n-butoxycarbonyl isocyanate. After 30 minutes of stirring at the same temperature, 1N sodium hydroxide aqueous solution was added dropwise thereto and the stirring was continued for 30 minutes at room temperature. After adding 1N hydrochloric acid, the solvent was evaporated, and the resulting residue was subjected to silica gel column chromatography to obtain 1.0 g of 1,3-bis[4-[(3,5-dioxo-1,2,4-oxadiazolidin-2-yl)methyl]phenoxy]benzene from fractions of chloroform-methanol (30:1) elution.

후처리

  1. temperaturecooling and in an atmosphere of argon
  2. additionwas added dropwise
  3. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-6fe3986684ff49c8bc654087af1a8eae
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05643931

반응 노트

불러오는 중…