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Methanimidic acid, N-phenyl-, ethyl ester → HCID 9820710、化合物

HRID 1729046
ノート
印刷プレビュー

反応式

HRID 1729046 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 9820710HCID 9820710、化合物収率 67.6%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-c682c3eb39564834a4ed678350945984
出典データセット
uspto-grants-1994_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05331005

反応ノート

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