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Triethylamine → HCID 178496794、化合物

HRID 444010
ノート
印刷プレビュー

反応式

HRID 444010 の反応式
C(N(CC)CC)C.Cl.Cl.[NH:10]([C:14]1[S:15][CH:16]=[C:17]([CH2:19][S:20][CH2:21][CH2:22][NH2:23])[N:18]=1)[C:11]([NH2:13])=[NH:12].[CH3:24][O:25][C:26](OC)=[N:27][C:28]#[N:29]>CO>[NH:10]([C:14]1[S:15][CH:16]=[C:17]([CH2:19][S:20][CH2:21][CH2:22][NH:23][C:26](=[N:27][C:28]#[N:29])[O:25][CH3:24])[N:18]=1)[C:11]([NH2:13])=[NH:12]
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 8471TriethylamineHCID 90604Carbonimidic acid, N-cyano-, dimethyl esterHCID 178478806HCID 178478806、化合物

生成物 1

HCID 178496794HCID 178496794、化合物収率 69%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Triethylamine (2.02 g.) was added to a suspension of 2-guanidino-4-[(2-aminoethyl)thiomethyl]thiazole dihydrochloride (3.04 g.) in methanol (30 ml.) stirred at room temperature. Dimethyl (N-cyanoimido)carbonate (1.14 g.) was added and the mixture was stirred at room temperature for 3 hours and then evaporated under reduced pressure. The residue was extracted with ethyl acetate (35 ml.) and the solution was washed with water (25 ml., 10 ml.) then dried (magnesium sulphate) and evaporated under reduced pressure to give 2-guanidino-4-[2-(3-cyano-2-methylisoureido)ethylthiomethyl]thiazole (2.16 g.). The n.m.r. spectrum in CDCl3 /d6 dimethyl sulphoxide using tetramethylsilane as internal standard had the following resonances (δ); 7.7 (1H, very broad); 6.7 (4H, broad); 6.4 (1H, singlet); 3.8 (3H, singlet); 3.6 (2H, singlet); 3.4 (obscured by H2O); 2.7 (2H, broad triplet).

後処理

  1. stirringthe mixture was stirred at room temperature for 3 hours
  2. customevaporated under reduced pressure
  3. extractionThe residue was extracted with ethyl acetate (35 ml.)
  4. washthe solution was washed with water (25 ml., 10 ml.)
  5. dry with materialthen dried (magnesium sulphate)
  6. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-df911ca1b65e429eb0eb86080bc705e8
出典データセット
uspto-grants-1981_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04262126

反応ノート

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