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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Acetic Acid → HCID 54553626, 화합물

HRID 27747
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인쇄 미리보기

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HRID 27747 반응식
[H-].[Na+].C[N:4](C)[CH:5]=[O:6].[C:8]([CH2:10][C:11]([NH2:13])=O)#[N:9].[Cl:14][C:15]1[CH:26]=[CH:25][C:18]2N=C(SC)C[S:22][C:17]=2[CH:16]=1.[C:27](O)(=O)C>O>[C:8]([C:10](=[C:11]1[CH2:27][C:18]2[CH:25]=[CH:26][C:15]([Cl:14])=[CH:16][C:17]=2[S:22][NH:13]1)[C:5]([NH2:4])=[O:6])#[N:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 176Acetic AcidHCID 6228DimethylformamideHCID 7898CyanoacetamideHCID 24758Sodium hydrideHCID 128710147-chloro-3-methylthio-2H-1,4-benzothiazine

생성물 1

HCID 54553626HCID 54553626, 화합물

시약·촉매·용매 1

HCID 962
Water
용매

실험 절차

To approximately 23 parts of sodium hydride in 4800 parts of N,N-dimethylformamide at room temperature under nitrogen is added, portionwise with stirring, 78 parts of 2-cyanoacetamide. Approximately 15 minutes later, a solution of 7-chloro-3-methylthio-2H-1,4-benzothiazine preparable as described in Part B of this example is slowly introduced, whereupon the reaction mixture is heated at 55° for 3 hours and then allowed to cool to room temperature overnight, stirring being continuous and the nitrogen atmosphere maintained throughout. The resultant mixture is acidified with glacial acetic acid and thereupon mixed with 3 volumes of water. Insoluble solids are filtered out and crystallized from aqueous N,N-dimethylformamide to give 2-cyano-2-(7-chloro-2,3-dihydro-4H-benzothiazin-3-ylidene)acetamide melting with decomposition in the range 150°-160°.

후처리

  1. customApproximately 15 minutes
  2. additionis slowly introduced, whereupon the reaction mixture
  3. temperatureis heated at 55° for 3 hours
  4. stirringstirring
  5. temperaturethe nitrogen atmosphere maintained throughout
  6. filtrationInsoluble solids are filtered out
  7. customcrystallized from aqueous N,N-dimethylformamide

출처 및 근거

ORD 기록
ord-f60f60817928463b923dba023c53c265
출처 데이터셋
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04223136

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