5-(((2-Aminoethyl)thio)methyl)-N,N-dimethyl-2-furanmethanamine → (3-Pyridyl)methylamino-1,2,5-thiadiazole 1-oxide

HRID 1980748노트

반응식

HRID 1980748 반응식
CO[C:3]1[C:7]([NH:8][CH2:9][C:10]2[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=2)=[N:6][S:5](=[O:16])[N:4]=1.CN(CC1OC(CSCCN)=CC=1)C>CO>[N:12]1[CH:13]=[CH:14][CH:15]=[C:10]([CH2:9][NH:8][C:7]2[CH:3]=[N:4][S:5](=[O:16])[N:6]=2)[CH:11]=1

참가 물질

4

반응물 2

HCID 1622035-(((2-Aminoethyl)thio)methyl)-N,N-dimethyl-2-furanmethanamineHCID 204020453-Methoxy-4-(3-pyridyl)methylamino-1,2,5-thiadiazole 1-oxide

생성물 1

HCID 20402190(3-Pyridyl)methylamino-1,2,5-thiadiazole 1-oxide

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

To the methanol solution of 3-methoxy-4-(3-pyridyl)methylamino-1,2,5-thiadiazole 1-oxide produced in Step A was added a solution of 2-[(5-dimethylaminomethyl-2-furyl)methylthio]ethylamine (4.0 g; 18.7 mmoles) in 30 ml of methanol. The reaction mixture was stirred at ambient temperatures for 18 hours and the solvent was removed in vacuo. The residue was placed on 500 g of silica gel (230-400 mesh) and purified by flash chromatography using a gradient elution of acetonitrile-methanol After combining the appropriate fractions, the title compound was obtained as an amber oil (4.25 g) containing one mole of methanol.

후처리

  1. customthe solvent was removed in vacuo
  2. custompurified by flash chromatography
  3. washa gradient elution of acetonitrile-methanol

출처 및 근거

ORD 기록
ord-d065fec3fd0e414eb40a8339d417849e
출처 데이터셋
uspto-grants-1985_04
특허 번호
US04510309

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