Tributylamine → HCID 178502897, 화합물

HRID 1584031노트

반응식

HRID 1584031 반응식
[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

참가 물질

7

반응물 4

HCID 7622Tributylamine2회HCID 24813Phosphorus oxychlorideHCID 521874O-Methylhydroxylamine hydrochlorideHCID 178525857HCID 178525857, 화합물

생성물 1

HCID 178502897HCID 178502897, 화합물수율 70.9%

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 12679Hexamethylphosphoramide용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-6f3e8c7ee6a74a208f3ba0531c60fb84
출처 데이터셋
uspto-grants-1985_11
특허 번호
US04555578

반응 노트

불러오는 중…