Sulfuric acid--4-methylpiperazine-1-carboximidamide (1/1) → HCID 25217526、化合物

HRID 910672ノート

反応式

HRID 910672 の反応式
CN([CH:4]=[N:5][C:6]([C:8]1[S:9][CH:10]=[C:11]([Br:13])[CH:12]=1)=O)C.S(O)(O)(=O)=O.[CH3:19][N:20]1[CH2:25][CH2:24][N:23]([C:26]([NH2:28])=[NH:27])[CH2:22][CH2:21]1.CC([O-])(C)C.[K+]>O1CCOCC1>[Br:13][C:11]1[CH:12]=[C:8]([C:6]2[N:28]=[C:26]([N:23]3[CH2:24][CH2:25][N:20]([CH3:19])[CH2:21][CH2:22]3)[N:27]=[CH:4][N:5]=2)[S:9][CH:10]=1

参加物

5

反応物 3

HCID 15564582Sulfuric acid--4-methylpiperazine-1-carboximidamide (1/1)HCID 23665647Potassium tert-butoxideHCID 67387591HCID 67387591、化合物

生成物 1

HCID 25217526HCID 25217526、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a solution of 4-bromo-thiophene-2-carboxylic acid dimethylamino-methyleneamide (261 mg, 1.0 mmol) in anhydrous 1,4-dioxane (8 mL) was added 4-methyl-piperazine-1-carboxamidine sulfate (95.6 mg, 0.25 mmol) and KOtBu (56.1 mg, 0.5 mmol). The resulting suspension was heated at reflux overnight under argon. After cooling, the reaction mixture was passed through a pad of diatomaceous earth, the filtrate was concentrated and the residue was purified by preparative TLC (2 M NH3 in MeOH/CH2Cl2) to yield the title compound as a yellowish solid.

後処理

  1. temperatureThe resulting suspension was heated
  2. temperatureat reflux overnight under argon
  3. temperatureAfter cooling
  4. concentrationthe filtrate was concentrated
  5. customthe residue was purified by preparative TLC (2 M NH3 in MeOH/CH2Cl2)

出典と根拠

ORDレコード
ord-de15b777da28428495725fd4bda6ff60
出典データセット
uspto-grants-2011_09
特許番号
US08022209B2

反応ノート

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