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Sulfuric Acid → 2-Methyl-3-oxo-6-(2-amino-ethyl)-3,4-dihydro-2H-1,4-benzoxazine

HRID 840375
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인쇄 미리보기

반응식

HRID 840375 반응식
[CH3:1][CH:2]1[C:7](=[O:8])[NH:6][C:5]2[CH:9]=[C:10]([CH:13]=[CH:14][N+:15]([O-])=O)[CH:11]=[CH:12][C:4]=2[O:3]1.S(=O)(=O)(O)O>[Pt](=O)=O.C(O)(=O)C>[CH3:1][CH:2]1[C:7](=[O:8])[NH:6][C:5]2[CH:9]=[C:10]([CH2:13][CH2:14][NH2:15])[CH:11]=[CH:12][C:4]=2[O:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 1118Sulfuric AcidHCID 54562509HCID 54562509, 화합물

생성물 1

HCID 226231212-Methyl-3-oxo-6-(2-amino-ethyl)-3,4-dihydro-2H-1,4-benzoxazine수율 52.7%

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매HCID 176Acetic Acid용매

실험 절차

2 g (8.5 mmol) of 2-methyl-3-oxo-6-(2-nitro-ethenyl)-3,4-dihydro-2H-1,4-benzoxazine is mixed with 80 ml of acetic acid and 1.6 ml of concentrated sulfuric acid and, after 200 mg of platinum dioxide is added, it is reduced in an autoclave. The catalyst is then suctioned off, and the batch is spun in until a dry state is reached. The remaining residue is chromatographed on silica gel (mobile solvent: isopropanol/ammonia). 923.5 mg (52.4%) of the described compound is obtained.

후처리

  1. customThe remaining residue is chromatographed on silica gel (mobile solvent: isopropanol/ammonia)

출처 및 근거

ORD 기록
ord-6e1e1810e5664fc9885352c48e5dcd44
출처 데이터셋
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06365736B1

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