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Ethanol → HCID 14347805, 화합물

HRID 2291765
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HRID 2291765 반응식
[CH2:1]([O:3][C:4]([CH2:6][N:7]1[C:12]2[CH:13]=[CH:14][C:15]([N+:17]([O-])=O)=[CH:16][C:11]=2[O:10][CH2:9][C:8]1=[O:20])=[O:5])[CH3:2].C(O)C.[H][H]>[C].[Pd].O1CCCC1>[NH2:17][C:15]1[CH:14]=[CH:13][C:12]2[N:7]([CH2:6][C:4]([O:3][CH2:1][CH3:2])=[O:5])[C:8](=[O:20])[CH2:9][O:10][C:11]=2[CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 702EthanolHCID 111501834-ethoxycarbonylmethyl-7-nitro-2H-1,4-benzoxazin-3(4H)-oneHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 14347805HCID 14347805, 화합물수율 74.7%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 8028Tetrahydrofuran
용매

실험 절차

A mixture of 4-ethoxycarbonylmethyl-7-nitro-2H-1,4-benzoxazin-3(4H)-one (30 g), 10% palladium-carbon (3 g) and ethanol (150 ml) was charged in an autoclave, and catalytically reduced under conditions of 20 kg/cm2 of hydrogen pressure and at a temperature of 60° C. to 70° C. Tetrahydrofuran was added thereto, and the liquor was filtered, then the filtrate was distilled under reduced pressure. Recrystallization of the resulting solid from ethanol gave the desired 7-amino-4-ethoxycarbonylmethyl-2H-1,4-benzoxazin-3(4H)-one (20 g). mp. 136°-137° C.

후처리

  1. additionwas charged in an autoclave
  2. filtrationthe liquor was filtered
  3. distillationthe filtrate was distilled under reduced pressure
  4. customRecrystallization of the resulting solid from ethanol

출처 및 근거

ORD 기록
ord-57289f45c3b54c60a49f565a41be1a19
출처 데이터셋
uspto-grants-1989_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04798620

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