Hydrazine hydrate (1:1) → HCID 21999979、化合物

HRID 1975909ノート

反応式

HRID 1975909 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 21999979HCID 21999979、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-981e5270e3fb4ab2b0124e442b29fe4d
出典データセット
uspto-grants-2001_05
特許番号
US06225310B1

反応ノート

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