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Sodium Hydroxide → N-[6-(n-butyl)-4H-1-benzothiopyran-4-on-3-yl)-oxalic acid monoamide

HRID 65468
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반응식

HRID 65468 반응식
C[N:2]([C:8]1[C:13](=[O:14])[C:12]2[CH:15]=[C:16]([CH2:19][CH2:20][CH2:21][CH3:22])[CH:17]=[CH:18][C:11]=2[S:10][CH:9]=1)[C:3]([C:5](N)=[O:6])=[O:4].[OH-:23].[Na+]>C(O)C.O>[CH2:19]([C:16]1[CH:17]=[CH:18][C:11]2[S:10][CH:9]=[C:8]([NH:2][C:3](=[O:4])[C:5]([OH:6])=[O:23])[C:13](=[O:14])[C:12]=2[CH:15]=1)[CH2:20][CH2:21][CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 86741043N-[6-(n-butyl)-4H-1-benzothiopyran-4-on-3-yl]-oxamide methyl ester

생성물 1

HCID 54266020N-[6-(n-butyl)-4H-1-benzothiopyran-4-on-3-yl)-oxalic acid monoamide

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

6.15 g (0.0193 mol) of N-[6-(n-butyl)-4H-1-benzothiopyran-4-on-3-yl]-oxamide methyl ester are stirred with a solution of 22.6 ml of 1N sodium hydroxide solution in 147 ml of ethanol and 970 ml of water for 2 hours at 70°. A small degree of cloudiness is then removed by filtration and the filtrate is acidified with hydrochloric acid, a crystalline product being precipitated. After cooling, the crystals are filtered with suction and washed first with water, then with ethanol and subsequently with ether. After drying there is obtained N-[6-(n-butyl)-4H-1-benzothiopyran-4-on-3-yl)-oxalic acid monoamide having a melting point of 208° (decomposition).

후처리

  1. customA small degree of cloudiness is then removed by filtration
  2. customa crystalline product being precipitated
  3. temperatureAfter cooling
  4. filtrationthe crystals are filtered with suction
  5. washwashed first with water
  6. customAfter drying there

출처 및 근거

ORD 기록
ord-033a7a6fcafa43958510dc1973ea2fb3
출처 데이터셋
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04614745

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