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Methanimidic acid, N-phenyl-, ethyl ester → HCID 9820710, 화합물

HRID 1729046
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HRID 1729046 반응식
[NH2:1][CH2:2][CH2:3][C:4]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([CH2:13][S:14]([NH:17][CH3:18])(=[O:16])=[O:15])[CH:11]=2)[NH:6][CH:5]=1.[C:19]1([N:25]=[CH:26]OCC)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>CC(C)=O>[C:19]1([NH:25][CH:26]=[N:1][CH2:2][CH2:3][C:4]2[C:12]3[C:7](=[CH:8][CH:9]=[C:10]([CH2:13][S:14]([NH:17][CH3:18])(=[O:15])=[O:16])[CH:11]=3)[NH:6][CH:5]=2)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 111236Methanimidic acid, N-phenyl-, ethyl esterHCID 9813988Didesmethyl sumatriptan

생성물 1

HCID 9820710HCID 9820710, 화합물수율 67.6%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

2.67 g (0.01 m) of 3-(2-aminoethyl)-1H-indole-5-yl-N-methyl methane sulphonamide and 10 mL of acetone were charged in a 25 mL round bottom flask. 1.64g (0.01 m) of ethyl N-phenylformimidate were added and the mixture was stirred at room temperature for 24 hours. When the reaction was deemed to have terminated, as per the TLC control (eluant: butanol/acetic acid/H2O 65/13/22) the acetone was concentrated to dryness and the oil obtained was crystallized from toluene. It was filtered, was washed with 10 mL of toluene and dried in a current of air at 50° C. to give 2.5 g of 3-[2-(N-phenylaminomethyleneamino)ethyl]-1H-indole-5-yl-N-methyl methane sulphonamide, in the form of a cream colored solid, representing a 67% yield. M.p.=72°-73° C.

후처리

  1. customto have terminated, as per the TLC control (eluant: butanol/acetic acid/H2O 65/13/22) the acetone
  2. concentrationwas concentrated to dryness
  3. customthe oil obtained
  4. customwas crystallized from toluene
  5. filtrationIt was filtered
  6. washwas washed with 10 mL of toluene
  7. customdried in a current of air at 50° C.

출처 및 근거

ORD 기록
ord-c682c3eb39564834a4ed678350945984
출처 데이터셋
uspto-grants-1994_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05331005

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