Stannous Chloride → 3-Hydrazino-4-methylbenzoic acid hydrochloride

HRID 1087

반응식

HRID 1087 반응식
[N:1]([O-])=O.[Na+].[NH2:5][C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][C:14]=1[CH3:15])[C:9]([OH:11])=[O:10].[Cl:16][Sn]Cl>O.Cl.CC(O)=O>[ClH:16].[NH:5]([C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][C:14]=1[CH3:15])[C:9]([OH:11])=[O:10])[NH2:1]

참가 물질

7

반응물 3

HCID 24479Stannous ChlorideHCID 755683-Amino-4-methylbenzoic acidHCID 23668193Sodium Nitrite

생성물 1

HCID 567775083-Hydrazino-4-methylbenzoic acid hydrochloride

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 313Hydrochloric Acid용매2회HCID 962Water용매

반응 조건

온도
0 °C

실험 절차

A solution of 2.74 g of NaNO2 in 28 ml of water is added over 30 minutes to a solution, cooled to -5° C., of 5 g of 3-amino-4-methylbenzoic acid in 120 ml of concentrated HCl and 40 ml AcOH, and the mixture is left stirring for 1 hour 20 minutes at 0° C. After cooling to -10° C., a solution of 27.6 g of SnCl2 ·2H2O in 28 ml of concentrated HCl is added slowly. After stirring for 1 hour at RT, filtration, washing of the precipitate with 5 ml of 1N HCl and drying over P2O5 under vacuum, 6.15 g of the expected product are obtained.

후처리

  1. waitthe mixture is left
  2. temperatureAfter cooling to -10° C.
  3. stirringAfter stirring for 1 hour at RT
  4. filtrationfiltration
  5. washwashing of the precipitate with 5 ml of 1N HCl
  6. dry with materialdrying over P2O5 under vacuum, 6.15 g of the expected product
  7. customare obtained

출처 및 근거

ORD 기록
ord-e46e69b904a7491db50b6afa5f24b6f5
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05723483

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