Hydrochloric Acid → HCID 178457562、化合物

HRID 236853ノート

反応式

HRID 236853 の反応式
[C:1]([NH:3][C:4]([NH:9][CH2:10][C:11]#[CH:12])=[N:5][CH2:6][CH2:7][SH:8])#[N:2].[Na].[CH3:14][C:15]1[N:16]=[CH:17][NH:18][C:19]=1[CH2:20]Cl.Cl>C(O)C>[C:1]([NH:3][C:4]([NH:5][CH2:6][CH2:7][S:8][CH2:20][C:19]1[NH:18][CH:17]=[N:16][C:15]=1[CH3:14])=[N:9][CH2:10][C:11]#[CH:12])#[N:2]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 5360545SodiumHCID 136182246N-Cyano-N'-propargyl-N"-(2-mercaptoethyl)guanidineHCID 178433264HCID 178433264、化合物

生成物 1

HCID 178457562HCID 178457562、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒3 回

実験手順

The ethanol solution of the product of step B, above, (about 10 m moles) was added to a solution of 0.46 sodium (0.02 g-atoms) in 10 ml ethanol at 4° C. under nitrogen. After 5 minutes, a solution of 1.67 g (10 m moles) of 4-methyl-5-chloromethylimidazole.HCl in 14 ml ethanol was added and the mixture was stirred at room temperature under nitrogen for 70 minutes. The reaction mixture was filtered through a bed of celite filter aid to remove the inorganic salts and the celite was washed with ethanol. The filtrate was evaporated to dryness and the product was purified by chromatography on a silica gel column (20 g silica, 3.2×4.5 cm bed) with ethanol-chloroform mixtures as the solvent. The ethanol content was gradually increased from 2 to 15%. The eluant was evaporated to dryness to give 1.906 g of crystalline product. Recrystallization from 2-propanol gave 1.49 g (54%) of the title product, m.p. 144°-145° C.

後処理

  1. filtrationThe reaction mixture was filtered through a bed of celite filter aid
  2. customto remove the inorganic salts
  3. washthe celite was washed with ethanol
  4. customThe filtrate was evaporated to dryness
  5. customthe product was purified by chromatography on a silica gel column (20 g silica, 3.2×4.5 cm bed) with ethanol-chloroform mixtures as the solvent
  6. temperatureThe ethanol content was gradually increased from 2 to 15%
  7. customThe eluant was evaporated to dryness

出典と根拠

ORDレコード
ord-6d75b10c751b46d99deede8647090de5
出典データセット
uspto-grants-1979_06
特許番号
US04158013

反応ノート

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