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Hydrochloric Acid → N-[(4,6-Dimethoxypyrimidin-2-yl)aminocarbonyl]-2-formylbenzenesulfonamide

HRID 1164174
ノート
印刷プレビュー

反応式

HRID 1164174 の反応式
[H-].COCCO[Al+]OCCOC.[Na+].[H-].N1CCOCC1.[CH3:21][O:22][C:23]1[CH:28]=[C:27]([O:29][CH3:30])[N:26]=[C:25]([NH:31][C:32]([NH:34][S:35]([C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][C:39]=2[C:44](OC)=[O:45])(=[O:37])=[O:36])=[O:33])[N:24]=1.Cl>O1CCCC1>[CH3:21][O:22][C:23]1[CH:28]=[C:27]([O:29][CH3:30])[N:26]=[C:25]([NH:31][C:32]([NH:34][S:35]([C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][C:39]=2[CH:44]=[O:45])(=[O:37])=[O:36])=[O:33])[N:24]=1
参加物反応条件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 8083MorpholineHCID 10810737N-[(4,6-Dimethoxypyrimidin-2-yl)aminocarbonyl]-2-methoxycarbonylbenzenesulfonamideHCID 21584525Sodium bis(2-methoxyethoxy)aluminiumhydride

生成物 1

HCID 13097377N-[(4,6-Dimethoxypyrimidin-2-yl)aminocarbonyl]-2-formylbenzenesulfonamide

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
-40 °C

実験手順

A mixture of 3.0 g of sodium bis(2-methoxyethoxy)aluminum hydride and 0.9 g of morpholine in 25 ml of dry tetrahydrofuran was cooled to -40° C. and 1.0 g of N-[(4,6-dimethoxypyrimidin-2-yl)aminocarbonyl]-2-methoxycarbonylbenzenesulfonamide was added. The resulting clear homogeneous solution was allowed to warm to room temperature over a period of 2 hours. Dilute hydrochloric acid was added and the mixture was extracted with methylene chloride. The organic extracts were washed, dried and evaporated. The crude product, which contained the desired aldehyde, the unreacted ester and the over-reduced alcohol, was purified by means of dry column chromatography. The purified product had a m.p. of 180° C.

後処理

  1. temperatureto warm to room temperature over a period of 2 hours
  2. extractionthe mixture was extracted with methylene chloride
  3. washThe organic extracts were washed
  4. customdried
  5. customevaporated
  6. customthe unreacted ester and the over-reduced alcohol, was purified by means of dry column chromatography

出典と根拠

ORDレコード
ord-2f724c0b47d04a6faf313899d03787b4
出典データセット
uspto-grants-1983_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04368069

反応ノート

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