Hydrochloric Acid → HCID 11092271、化合物

HRID 2187503ノート

反応式

HRID 2187503 の反応式
C1CCN2C(=NCCC2)CC1.[NH2:12][S:13]([C:16]1[CH:25]=[C:24]([CH2:26][CH2:27][NH:28][C:29]([O:31][CH3:32])=[O:30])[CH:23]=[CH:22][C:17]=1[C:18]([O:20][CH3:21])=[O:19])(=[O:15])=[O:14].[CH3:33][O:34][C:35]1[CH:40]=[C:39]([O:41][CH3:42])[N:38]=[C:37]([N:43](C2C=CC=CC=2)[C:44](=O)[O-:45])[N:36]=1.Cl>C(#N)C.O.C(OCC)C>[CH3:42][O:41][C:39]1[CH:40]=[C:35]([O:34][CH3:33])[N:36]=[C:37]([NH:43][C:44]([NH:12][S:13]([C:16]2[CH:25]=[C:24]([CH2:26][CH2:27][NH:28][C:29]([O:31][CH3:32])=[O:30])[CH:23]=[CH:22][C:17]=2[C:18]([O:20][CH3:21])=[O:19])(=[O:14])=[O:15])=[O:45])[N:38]=1

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 11034420HCID 11034420、化合物HCID 22104197HCID 22104197、化合物

生成物 1

HCID 11092271HCID 11092271、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒HCID 6342Acetonitrile溶媒

実験手順

0.26 ml (1.7 mmol) of DBU was added dropwise to a suspension of 0.54 g (1.7 mmol) of methyl 2-aminosulfonyl-4-[2-(methoxycarbonylamino)ethyl]benzoate and 0.47 g (1.7 mmol) of N-(4,6-dimethoxypyrimidin-2-yl)phenylcarbamate in 15 ml of acetonitrile. After 2 h, the mixture was diluted with water and diethyl ether and acidified with HCl to pH 1-2, and the product precipitated was removed by filtration, washed with water and diethyl ether and dried. Yield: 0.47 g (55.6%) of methyl 2-[(4,6-dimethoxypyrimidin-2-yl)aminocarbonylaminosulfonyl]-4-[2-(methoxycarbonylamino)ethyl]benzoate of m.p.: 165-169° C./decomp.

後処理

  1. customthe product precipitated
  2. customwas removed by filtration
  3. washwashed with water and diethyl ether
  4. customdried

出典と根拠

ORDレコード
ord-20ef74d6db274daeb2b77f3068a1f954
出典データセット
uspto-grants-2002_06
特許番号
US06410483B1

反応ノート

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