Methylamine → 5-amino-N-methyl-1,3,4-thiadiazole-2-sulfonamide

HRID 731496

반응식

HRID 731496 반응식
[CH3:1][NH2:2].C([NH:6][C:7]1[S:11][C:10]([S:12](Cl)(=[O:14])=[O:13])=[N:9][N:8]=1)(=O)C>C1COCC1>[CH3:1][NH:2][S:12]([C:10]1[S:11][C:7]([NH2:6])=[N:8][N:9]=1)(=[O:14])=[O:13]

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 128944515-(Acetylamino)-1,3,4-thiadiazole-2-sulfonyl chloride

생성물 1

HCID 674836825-amino-N-methyl-1,3,4-thiadiazole-2-sulfonamide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Methylamine (2M in THF, 40 mmol) was added to a suspension of 5-acetylamino-1,3,4-thiadiazole-2-sulfonyl chloride (10 mmol) (prepared as described in Bioorg. Med. Chem. 5, 515, 1997) in THF (10 mL) at −20° C. The mixture was stirred at room temperature over night and evaporated to dryness. The crude methylsulfonamide was suspended in EtOH (15 mL) and added 4N HCl in dioxane (15 mL) and heated for 4 h at 80° C. and then cooled to room temperature and evaporated to dryness to give crude 5-amino-1,3,4-thiadiazole-2-sulfonic acid methylamide.

후처리

  1. customevaporated to dryness
  2. additionadded 4N HCl in dioxane (15 mL)
  3. temperatureheated for 4 h at 80° C.
  4. temperaturecooled to room temperature
  5. customevaporated to dryness

출처 및 근거

ORD 기록
ord-182dba6a50ef45dc97d03ccfdac3c922
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07582769B2

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