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Hydrochloric Acid → N-[(4,6-Dimethoxypyrimidin-2-yl)aminocarbonyl]-3-(methoxymethyl)thiophene-2-sulfonamide

HRID 1252348
ノート
印刷プレビュー

反応式

HRID 1252348 の反応式
[CH3:1][O:2][CH2:3][C:4]1[CH:8]=[CH:7][S:6][C:5]=1[S:9]([NH2:12])(=[O:11])=[O:10].[CH3:13][O:14][C:15]1[CH:20]=[C:19]([O:21][CH3:22])[N:18]=[C:17]([NH:23][C:24](=O)[O:25]C2C=CC=CC=2)[N:16]=1.N12CCCN=C1CCCCC2.Cl>C(#N)C>[CH3:22][O:21][C:19]1[CH:20]=[C:15]([O:14][CH3:13])[N:16]=[C:17]([NH:23][C:24]([NH:12][S:9]([C:5]2[S:6][CH:7]=[CH:8][C:4]=2[CH2:3][O:2][CH3:1])(=[O:11])=[O:10])=[O:25])[N:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 10945667Carbamic acid, N-(4,6-dimethoxy-2-pyrimidinyl)-, phenyl esterHCID 139132183-(Methoxymethyl)thiophene-2-sulfonamide

生成物 1

HCID 13913192N-[(4,6-Dimethoxypyrimidin-2-yl)aminocarbonyl]-3-(methoxymethyl)thiophene-2-sulfonamide

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒

実験手順

To 0.41 g of 3-(methoxymethyl)thiophene-2-sulfonamide and 0.55 g of phenyl N-(4,6-dimethoxypyrimidin-2-yl)carbamate in 20 mL of acetonitrile is added 0.3 mL of 1,8-diazabicyclo-[5.4.0]undec-7-ene (DBU). After being stirred for 2 hours at ambient temperature and pressure, the reaction mass is poured onto 25-50 g of ice and the resultant mixture acidified to pH 3 by the addition of hydrochloric acid. The desired solid product can be isolated by filtration. Alternatively, it can be extracted into methylene chloride which is then dried over magnesium sulfate, filtered and evaporated to dryness to yield the desired product is sufficiently pure form for the purposes of this invention.

後処理

  1. customThe desired solid product can be isolated by filtration
  2. extractionAlternatively, it can be extracted into methylene chloride which
  3. dry with materialis then dried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated to dryness

出典と根拠

ORDレコード
ord-c1ee071ccd054deabe438b63731c71b7
出典データセット
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04743290

反応ノート

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