Hydrochloric Acid → Methyl 2-[[[[(4-Methoxy-6-methyl-1,3,6-triazin-2-yl)amino]carbonyl]amino]sulfonyl]-1-methyl-1H-pyrrole-3-carboxylate

HRID 829

反応式

HRID 829 の反応式
[NH2:1][S:2]([C:5]1[N:6]([CH3:14])[CH:7]=[CH:8][C:9]=1[C:10]([O:12][CH3:13])=[O:11])(=[O:4])=[O:3].C[O:16][C:17]1N=C(C)[N:20]=[C:19]([NH:24][C:25](=O)[O:26][C:27]2C=CC=CC=2)[N:18]=1.C1CCN2[C:37](=[N:38][CH2:39]CC2)CC1.Cl>C(#N)C.O>[CH3:27][O:26][C:25]1[N:24]=[C:19]([NH:18][C:17]([NH:1][S:2]([C:5]2[N:6]([CH3:14])[CH:7]=[CH:8][C:9]=2[C:10]([O:12][CH3:13])=[O:11])(=[O:4])=[O:3])=[O:16])[NH:20][N:38]([CH3:39])[CH:37]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 11448329Carbamic acid, (4-methoxy-6-methyl-1,3,5-triazin-2-yl)-, phenyl esterHCID 15790330Methyl 2-(aminosulfonyl)-1-methyl-1H-pyrrole-3-carboxylate

生成物 1

HCID 19693847Methyl 2-[[[[(4-Methoxy-6-methyl-1,3,6-triazin-2-yl)amino]carbonyl]amino]sulfonyl]-1-methyl-1H-pyrrole-3-carboxylate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

実験手順

Methyl 2-(aminosulfonyl)-1-methyl-1H-pyrrole-3-carboxylate (0.10 g, 0.46 mmol) and 0.13 g (0.50 mmol) of phenyl (4-methoxy-6-methyl-1,3,5-triazin-2-yl)carbamate were combined in 2 mL of acetonitrile and 0.075 mL of DBU was added and the resulting amber solution was stirred at ambient temperature for 30 min. The reaction mixture was diluted with 15 mL of water and acidified with 0.5 mL 1N HCl and the resulting precipitate was collected by filtration and rinsed successively with water and ether, then dried to afford 0.13 g oil the title compound as a white solid, m.p. 189°-190° C. (dec).

後処理

  1. filtrationthe resulting precipitate was collected by filtration
  2. washrinsed successively with water and ether
  3. customdried

出典と根拠

ORDレコード
ord-a5a19d2e3ccc4cb7bff13f06f043ffc0
出典データセット
uspto-grants-1998_03
特許番号
US05723410

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