Hydrochloric Acid → 2-Amino-4-[2-(hydrazinoimino-methyl)hydrazino]-butanoic acid

HRID 1109027

반응식

HRID 1109027 반응식
[NH2:1][C@H:2]([C:7]([OH:9])=[O:8])[CH2:3][CH2:4]ON.CS/[C:12](/[NH2:15])=[N:13]/[NH2:14].I.[N:17]#[N:18].Cl>[OH-].[Na+]>[NH2:1][CH:2]([CH2:3][CH2:4][NH:14][NH:13][CH:12]=[N:15][NH:17][NH2:18])[C:7]([OH:9])=[O:8]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 947Nitrogen2회HCID 441443L-CanalineHCID 6508896Methyl hydrazinecarbimidothioate hydroiodide

생성물 1

HCID 540366152-Amino-4-[2-(hydrazinoimino-methyl)hydrazino]-butanoic acid

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

반응 조건

온도
4 °C

실험 절차

Mix canaline (2.65 g, 20 mmol) and S-methylisothiosemicarbazide hydroiodide (4.66 g, 20 mmol) in 1M NaOH (40 ml) and stir under a blanket N2 at 40° C. for 48 hours. Neutralize the reaction with 1M HCl and blow to a residue with a stream of N2. Apply the residue to a Dowex AG50-X8 column and elute with 0.2M NH4OH. Lyophilize the fractions containing the desired product and take up the resulting solid in water (20 ml). Add flavianic acid (3.2 g) in water (20 ml) and cool the solution to 4° C. for 16 hours. Filter the resulting solid and crystallize to yield the title compound.

후처리

  1. washApply the residue to a Dowex AG50-X8 column and elute with 0.2M NH4OH
  2. additioncontaining the desired product
  3. filtrationFilter the resulting solid
  4. customcrystallize

출처 및 근거

ORD 기록
ord-c8cda447d7c7482da4b25906b25fe5f4
출처 데이터셋
uspto-grants-1994_06
특허 번호
US05318992

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