Tributylamine → HCID 178502897、化合物

HRID 1584031ノート

反応式

HRID 1584031 の反応式
[SH:1][C:2]1[N:6]([CH2:7][C:8]([OH:10])=O)[N:5]=[N:4][N:3]=1.C(N(CCCC)CCCC)CCC.P(Cl)(Cl)(Cl)=O.Cl.[CH3:30][O:31][NH2:32]>C(#N)C.CN(P(N(C)C)(N(C)C)=O)C>[CH3:30][O:31][NH:32][C:8](=[O:10])[CH2:7][N:6]1[C:2]([SH:1])=[N:3][N:4]=[N:5]1

参加物

7

反応物 4

HCID 7622Tributylamine2 回HCID 24813Phosphorus oxychlorideHCID 521874O-Methylhydroxylamine hydrochlorideHCID 178525857HCID 178525857、化合物

生成物 1

HCID 178502897HCID 178502897、化合物収率 70.9%

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 12679Hexamethylphosphoramide溶媒

実験手順

To an ice cold solution of 5-mercapto-1H-tetrazole-1-acetic acid (160 mg) in acetonitrile (3.2 ml) are added tri-n-butylamine (476 μl) and phosphorus oxychloride (183 μl). After 80 minutes' stirring, a solution of methoxyamine hydrochloride (167 mg) and tri-n-butylamine (476 μl) in hexamethylphosphorotriamide is added to the above solution. After another 1 hour's stirring at 0° C., the mixture is extracted with 5% aqueous sodium hydrogen carbonate (40 ml). The extract solution is washed with ethyl acetate, acidified with concentrated hydrochloric acid to pH 2.5, saturated with sodium chloride and extracted with methyl ethyl ketone. The extract is dried over magnesium sulfate and concentrated to give 5-mercapto-1H-tetrazole-1-acetohydroxamic acid methyl ester (134 mg). mp. 165°-167° C. (decomp.).

後処理

  1. stirringAfter another 1 hour's stirring at 0° C.
  2. extractionthe mixture is extracted with 5% aqueous sodium hydrogen carbonate (40 ml)
  3. washThe extract solution is washed with ethyl acetate
  4. extractionextracted with methyl ethyl ketone
  5. dry with materialThe extract is dried over magnesium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-6f3e8c7ee6a74a208f3ba0531c60fb84
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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