Hydrazine hydrate (1:1) → HCID 21999979, 화합물

HRID 1975909노트

반응식

HRID 1975909 반응식
[C:1]([C:3]1[C:4]([S:13](=[O:16])(=[O:15])[NH2:14])=[C:5]([C:9](OC)=[O:10])[S:6][C:7]=1[CH3:8])#[N:2].NC1C(C#N)=C(C)SC=1C(OC)=O.O.[NH2:31][NH2:32]>C(O)C>[C:1]([C:3]1[C:4]([S:13]([NH2:14])(=[O:16])=[O:15])=[C:5]([C:9]([NH:31][NH2:32])=[O:10])[S:6][C:7]=1[CH3:8])#[N:2]

참가 물질

5

반응물 3

HCID 24654Hydrazine hydrate (1:1)HCID 15565691Methyl 3-amino-4-cyano-5-methylthiophene-2-carboxylateHCID 21999999HCID 21999999, 화합물

생성물 1

HCID 21999979HCID 21999979, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Methyl 4-cyano-5-methyl-3-sulfamoyl-thiophene-2-carboxylate (2.9 g), prepared from methyl 3-amino-4-cyano-5-methyl-thiophene-2-carboxylate in analogy with known procedures, e.g. F. Junquera et al., Eur.J.Med.Chem. 23, 329 (1988), was suspended in 10 ml of ethanol. Hydrazine monohydrate (2 ml) was added and the mixture was stirred for 1 h at room temperature and then evaporated. The oily residue (3.3 g) was triturated with 10 ml of water and the precipitating crystals were collected by filtration, washed with water and dried to give the title compoundas yellow crystals (yield 1.62 g); m.p. 186-91° C.; 1H-NMR (DMSO-d6), δ(ppm): 7.25 (br, 5H, NH/NH2), 2.51 (s, 3H, CH3).

후처리

  1. customevaporated
  2. customThe oily residue (3.3 g) was triturated with 10 ml of water
  3. filtrationthe precipitating crystals were collected by filtration
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-981e5270e3fb4ab2b0124e442b29fe4d
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06225310B1

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