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

HRID 1249137

반응식

HRID 1249137 반응식
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

참가 물질

6

반응물 4

HCID 962WaterHCID 7090PhenidoneHCID 8471TriethylamineHCID 15225519N-Bromomethylsaccharin

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e33fd103d6a4416f9e7bf1ca6b56b815
출처 데이터셋
uspto-grants-1986_12
특허 번호
US04629683

연결된 노트

불러오는 중…