3,4-Dimethoxy-1,2,5-thiadiazole 1-oxide → 3-[4-(3-Amino-5-bromopyrid-2-yl)butylamino]-4-methoxy-1,2,5-thiadiazole-1-oxide

HRID 371406노트

반응식

HRID 371406 반응식
[CH3:1][O:2][C:3]1[C:7](OC)=[N:6][S:5](=[O:10])[N:4]=1.[NH2:11][C:12]1[C:13]([CH2:19][CH2:20][CH2:21][CH2:22][NH2:23])=[N:14][CH:15]=[C:16]([Br:18])[CH:17]=1>CO>[NH2:11][C:12]1[C:13]([CH2:19][CH2:20][CH2:21][CH2:22][NH:23][C:7]2[C:3]([O:2][CH3:1])=[N:4][S:5](=[O:10])[N:6]=2)=[N:14][CH:15]=[C:16]([Br:18])[CH:17]=1

참가 물질

4

반응물 2

HCID 129139473,4-Dimethoxy-1,2,5-thiadiazole 1-oxideHCID 145374593-Amino-5-bromo-(4-aminobutyl)pyridine

생성물 1

HCID 159623603-[4-(3-Amino-5-bromopyrid-2-yl)butylamino]-4-methoxy-1,2,5-thiadiazole-1-oxide수율 74%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

A solution of 3,4-dimethoxy-1,2,5-thiadiazole-1-oxide (0.995 g) in methanol (25 ml) was reacted with a solution of 3-amino-5-bromo-(4-aminobutyl)pyridine (1.5 g) in methanol (25 ml) at room temperature for 3 hours. The solvent was removed in vacuo and the residue was chromatographed on silica in ethanol to give an oil which was triturated with ether and recrystallised from ethanol/ether to give 3-[4-(3-amino-5-bromopyrid-2-yl)butylamino]-4-methoxy-1,2,5-thiadiazole-1-oxide (1.7 g) m.p. 118°-120° C.

후처리

  1. customThe solvent was removed in vacuo
  2. customthe residue was chromatographed on silica in ethanol
  3. customto give an oil which
  4. customwas triturated with ether
  5. customrecrystallised from ethanol/ether

출처 및 근거

ORD 기록
ord-b242893aab1c434bad0799f465662436
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04532252

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