Methanimidamide, hydrochloride (1:1) → HCID 135767899, 화합물

HRID 2405757노트

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HRID 2405757 반응식
[Cl:1][C:2]1[CH:10]=[C:6]([C:7]([OH:9])=O)[C:5]([NH2:11])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].Cl.[CH:16](N)=[NH:17]>>[Cl:1][C:2]1[CH:10]=[C:6]2[C:5](=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13])[N:11]=[CH:16][NH:17][C:7]2=[O:9]

참가 물질

3

반응물 2

HCID 10313058Methanimidamide, hydrochloride (1:1)HCID 214739642-Amino-5-chloro-4-nitrobenzoic acid

생성물 1

HCID 135767899HCID 135767899, 화합물수율 84.2%

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온도
205 °C

실험 절차

A mixture of 5-chloro-4-nitroanthranilic acid (8.7 g, 0.040 mol) and formamidine hydrochloride (4.9 g, 60 mmol) were ground to a fine, intimate powder using a mortar and pestle. The mixture was transferred into a 250 mL round bottomed flask and immersed in an oil bath maintained at 205° C. After 40 min, LCMS analysis of the reaction mixture showed mass corresponding to the product. The reaction mixture was cooled and the crude product was crushed into pieces and washed several times with saturated NaHCO3 (300 mL) and water (200 mL). The solid was air dried and triturated with a minimum amount of MeOH (20 mL) to obtain 6-chloro-7-nitroquinazoline-4-one (7.6 g, 83%) as a tan powder.

후처리

  1. customThe mixture was transferred into a 250 mL round bottomed flask
  2. customimmersed in an oil bath
  3. temperatureThe reaction mixture was cooled
  4. washwashed several times with saturated NaHCO3 (300 mL) and water (200 mL)
  5. customdried
  6. customtriturated with a minimum amount of MeOH (20 mL)

출처 및 근거

ORD 기록
ord-9758a1b25dfe40a9a7b7402495333a4e
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08809326B2

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