Sulfuric acid--4-methylpiperazine-1-carboximidamide (1/1) → HCID 25217526, 화합물

HRID 910672노트

반응식

HRID 910672 반응식
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

참가 물질

5

반응물 3

HCID 15564582Sulfuric acid--4-methylpiperazine-1-carboximidamide (1/1)HCID 23665647Potassium tert-butoxideHCID 67387591HCID 67387591, 화합물

생성물 1

HCID 25217526HCID 25217526, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-de15b777da28428495725fd4bda6ff60
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022209B2

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