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Sodium Hydroxide → HCID 178484432、化合物

HRID 1194322
ノート
印刷プレビュー

反応式

HRID 1194322 の反応式
[CH3:1][N:2]([CH3:14])[C:3]([C:5]1[O:6][C:7]([C:10](=O)[CH2:11]Br)=[CH:8][CH:9]=1)=[O:4].[C:15]([NH:18][C:19]([NH2:21])=[S:20])(=[NH:17])[NH2:16].[OH-].[Na+]>CC(C)=O>[NH:18]([C:19]1[S:20][CH:11]=[C:10]([C:7]2[O:6][C:5]([C:3](=[O:4])[N:2]([CH3:14])[CH3:1])=[CH:9][CH:8]=2)[N:21]=1)[C:15]([NH2:17])=[NH:16]
参加物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 14798Sodium HydroxideHCID 15615543HCID 15615543、化合物HCID 178513045HCID 178513045、化合物2 回

生成物 1

HCID 178484432HCID 178484432、化合物収率 17.9%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 2.6 g. (0.01 mole) of N,N-dimethyl5-(2-bromoacetyl)furan-2-carboxamide, 1.18 g. (0.01 mole) of guanylthiourea and 100 ml. of acetone was stirred at room temperature for 4 hours. An additional 354 mg. of guanylthiourea was added and stirring was continued for 3 days. The reaction mixture was filtered, and the residue was washed with acetone and then dissolved in water. The solution thus obtained was made alkaline using 10% sodium hydroxide solution and extracted with ethyl acetate. The extracts were dried (MgSO4) and concentrated in vacuo to give a first crop of the title compound (500 mg.). The aqueous phase from the extraction was further basified (to pH 14) and extracted with n-butanol. Evaporation of the n-butanol gave a second crop of the title compound (900 mg.). The two crops of the title compound were combined and recrystallized from aqueous ethanol, giving 550 mg. of a brown solid, mp. 252°-253.5° C. (dec). Two additional samples of the title compound were obtained from the recrystallization mother liquors: 190 mg. mp 249°-252° C.; 91 mg., mp 248°-251° C.

後処理

  1. additionA mixture of 2.6 g
  2. filtrationThe reaction mixture was filtered
  3. washthe residue was washed with acetone
  4. dissolutiondissolved in water
  5. customThe solution thus obtained
  6. extractionextracted with ethyl acetate
  7. dry with materialThe extracts were dried (MgSO4)
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-60e623d036214959bb2984a47bd03ef1
出典データセット
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04814341

反応ノート

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