Ammonium Chloride → 1013117-35-5

HRID 2405758노트

반응식

HRID 2405758 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[N+:12]([O-])=O)[N:8]=[CH:7][NH:6][C:5]2=[O:15].[NH4+].[Cl-]>CO.O.[Fe]>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[NH2:12])[N:8]=[CH:7][NH:6][C:5]2=[O:15]

참가 물질

6

반응물 2

HCID 25517Ammonium ChlorideHCID 135767899HCID 135767899, 화합물

생성물 1

HCID 1360138721013117-35-5수율 100.7%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
65 °C

실험 절차

To a suspension of 6-chloro-7-nitroquinazoline-4-one (7.5 g, 33 mmol) in MeOH (250 mL) was added NH4Cl (17.7 g, 0.33 mol) dissolved in water (75 mL). Iron powder (18.5 g, 330 mmol) was added and the suspension was heated at 65° C. for 2 h. The warm reaction mixture was filtered over diatomaceous earth and washed several times with THF (1 L) and methanol (500 mL). The filtrate was concentrated, washed with water and dried under vacuum at 50° C. to afford the title compound (6.5 g, 90%) as a brown solid. ESI-MS m/z 196 [C8H6ClN3O+H]+.

후처리

  1. customThe warm reaction mixture
  2. filtrationwas filtered over diatomaceous earth
  3. washwashed several times with THF (1 L) and methanol (500 mL)
  4. concentrationThe filtrate was concentrated
  5. washwashed with water
  6. customdried under vacuum at 50° C.

출처 및 근거

ORD 기록
ord-a111bca80fd34374af0fd0545523b698
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08809326B2

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