Hydrochloric Acid → 5-mercapto-1H-tetrazole-1-propionohydroxamic acid methyl ester

HRID 1584036ノート

反応式

HRID 1584036 の反応式
[SH:1][C:2]1[N:6]([CH2:7][CH2:8][C:9]([OH:11])=O)[N:5]=[N:4][N:3]=1.Cl.[CH3:13][O:14][NH2:15].C(N(CC)CC)C.Cl>CN(C)C=O>[CH3:13][O:14][NH:15][C:9](=[O:11])[CH2:8][CH2:7][N:6]1[C:2]([SH:1])=[N:3][N:4]=[N:5]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 521874O-Methylhydroxylamine hydrochlorideHCID 178525591HCID 178525591、化合物

生成物 1

HCID 1785028945-mercapto-1H-tetrazole-1-propionohydroxamic acid methyl ester収率 98.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
0 °C

実験手順

To an ice cold and stirred solution of 5-mercapto-1H-tetrazole-1-propionic acid (1.04 g) in N,N-dimethylformamide (60 ml) is added N,N'-carbonyldiimidazole (1.16 g). After stirring for 15 minutes at 0° C., the mixture is mixed with a solution of methoxyamine hydrochloride (600 mg) and triethylamine (720 mg) in N,N-dimethylformamide (6 ml) and stirred for 1 hour at 0° C. The reaction mixture is poured into diluted hydrochloric acid and extracted with a mixture of ethyl acetate and methyl ethyl ketone (2:1). The solvent is evaporated from the extract to leave crystalline 5-mercapto-1H-tetrazole-1-propionohydroxamic acid methyl ester (1.2 g). mp. 170°-171° C. (decomp.).

後処理

  1. stirringstirred for 1 hour at 0° C
  2. extractionextracted with a mixture of ethyl acetate and methyl ethyl ketone (2:1)
  3. customThe solvent is evaporated from the
  4. extractionextract

出典と根拠

ORDレコード
ord-32bb0034c01645df8dd473f3d9cabf60
出典データセット
uspto-grants-1985_11
特許番号
US04555578

反応ノート

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