Water → N-(1-phenyl-3-pyrazolidinone-2-ylmethyl)saccharin

HRID 1249137ノート

反応式

HRID 1249137 の反応式
Br[CH2:2][N:3]1[C:13](=[O:14])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[S:4]1(=[O:6])=[O:5].[C:15]1([N:21]2[CH2:25][CH2:24][C:23](=[O:26])[NH:22]2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C(N(CC)CC)C.O>O1CCCC1>[C:15]1([N:21]2[CH2:25][CH2:24][C:23](=[O:26])[N:22]2[CH2:2][N:3]2[C:13](=[O:14])[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[S:4]2(=[O:6])=[O:5])[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

参加物

6

反応物 4

HCID 962WaterHCID 7090PhenidoneHCID 8471TriethylamineHCID 15225519N-Bromomethylsaccharin

生成物 1

HCID 20224974N-(1-phenyl-3-pyrazolidinone-2-ylmethyl)saccharin収率 89.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

N-Bromomethylsaccharin (13.8 g), 1-phenyl-3-pyrazolidinone (11.9 g) and triethylamine (5.5 g) were dissolved in tetrahydrofuran (200 ml), and stirred in a stream of nitrogen at room temperature for 2 hours. The reaction mixture was added to water (200 ml), and extracted with 100 ml each of ethyl acetate two times. After drying the extract over anhydrous Glauber's salt, the solvent was distilled away. The thus obtained crude product was recrystallized from ethyl acetate to yield 16 g of N-(1-phenyl-3-pyrazolidinone-2-ylmethyl)saccharin (Compound (I)-(18)). Melting Point: 209°-213° C.

後処理

  1. extractionextracted with 100 ml each of ethyl acetate two times
  2. customAfter drying the
  3. extractionextract over anhydrous Glauber's salt
  4. distillationthe solvent was distilled away
  5. customThe thus obtained crude product
  6. customwas recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-e33fd103d6a4416f9e7bf1ca6b56b815
出典データセット
uspto-grants-1986_12
特許番号
US04629683

反応ノート

読み込み中…