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Carbamimidic acid, methyl ester, sulfate (1:1) → HCID 178494253、化合物

HRID 1169810
ノート
印刷プレビュー

反応式

HRID 1169810 の反応式
CC[O-].[Na+].S(O)(O)(=O)=O.[CH3:10][O:11][C:12]([NH2:14])=[NH:13].C[CH2:16][CH:17]([C:22](OCC)=[O:23])[C:18](OC)=[O:19]>C(O)C>[CH3:10][O:11][C:12]1[N:14]=[C:18]([OH:19])[C:17]([CH3:16])=[C:22]([OH:23])[N:13]=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

5

反応物 3

HCID 169039Carbamimidic acid, methyl ester, sulfate (1:1)HCID 2723922Sodium ethoxideHCID 5088009HCID 5088009、化合物

生成物 1

HCID 178494253HCID 178494253、化合物収率 72.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

反応条件

温度
0 °C

実験手順

13.8 g (200 mmoles) of sodium ethylate is added to a solution of 10 g (58 mmoles) of methoxyformamidine sulphate in 100 ml of ethanol cooled down to 0° C. and the mixture is stirred for 15 minutes; then a solution of 9 ml (52 mmoles) of diethyl methyl malonate in 50 ml of ethanol is added followed by stirring overnight at ambient temperature. The reaction mixture is evaporated to dryness under reduced pressure (2 kPa). The residue is taken up in 100 ml of a saturated solution of sodium chloride and extracted with 800 and 200 ml of n-butanol. The organic phases are dried over sodium sulphate, filtered and evaporated to dryness under reduced pressure (2 kPa), 5.9 g of expected product is obtained in the form of a white solid.

後処理

  1. stirringby stirring overnight at ambient temperature
  2. customThe reaction mixture is evaporated to dryness under reduced pressure (2 kPa)
  3. extractionextracted with 800 and 200 ml of n-butanol
  4. dry with materialThe organic phases are dried over sodium sulphate
  5. filtrationfiltered
  6. customevaporated to dryness under reduced pressure (2 kPa)

出典と根拠

ORDレコード
ord-eac0e27347984584811ec29c59307567
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07825119B2

反応ノート

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