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Hydrazine hydrate (1:1) → HCID 57470539, 화합물

HRID 1270158
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HRID 1270158 반응식
O.[NH2:2][NH2:3].[CH3:4][O:5][C:6]([C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[N:14]=[C:13](Cl)[C:12]([Cl:19])=[N:11]2)=[O:7]>CO>[CH3:4][O:5][C:6]([C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[N:14]=[C:13]([NH:2][NH2:3])[C:12]([Cl:19])=[N:11]2)=[O:7]
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)2회HCID 13799594Methyl 2,3-dichloroquinoxaline-6-carboxylate

생성물 1

HCID 57470539HCID 57470539, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

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온도
0 °C

실험 절차

Hydrazine monohydrate (0.26 mL) was added dropwise to a suspension of 2,3-dichloro-quinoxaline-6-carboxylic acid methyl ester (1.2 g) in methanol (10 mL) at −10° C. After three hrs. at this temperature, an additional portion of hydrazine monohydrate (0.26 mL) was added, and the resulting mixture was stirred at 0° C. for three hrs., and then for one hr. at 23° C. The suspension was filtered, and the solids were washed with MeOH. Flash column chromatography provided a residue that was recrystallized from MeOH to provide 3-chloro-2-hydrazino-quinoxaline-6-carboxylic acid methyl ester as a yellow solid. MS (M+H)+=253.2.

후처리

  1. wait, and then for one hr
  2. customat 23° C
  3. filtrationThe suspension was filtered
  4. washthe solids were washed with MeOH
  5. customFlash column chromatography provided a residue that
  6. customwas recrystallized from MeOH

출처 및 근거

ORD 기록
ord-aa2499738a664bf9816f1d4e2875dc1a
출처 데이터셋
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07202245B2

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