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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 15718785, 화합물 → HCID 178488097, 화합물

HRID 2166125
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HRID 2166125 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[NH:10][C:11]([NH:13][CH:14]1[CH2:19][CH2:18][N:17]([CH3:20])[CH2:16][CH2:15]1)=S>[Hg]=O.O1CCCC1>[CH3:9][O:8][C:5]1[CH:6]=[CH:7][C:2]2[NH:1][C:11]([NH:13][CH:14]3[CH2:19][CH2:18][N:17]([CH3:20])[CH2:16][CH2:15]3)=[N:10][C:3]=2[CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 15718785HCID 15718785, 화합물

생성물 1

HCID 178488097HCID 178488097, 화합물수율 100%

시약·촉매·용매 2

HCID 30856Mercuric oxide촉매HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 44 parts of N-(2-amino-5-methoxyphenyl)-N'-(1-methyl-4-piperidinyl)thiourea, 38.9 parts of mercury(II) oxide and 270 parts of tetrahydrofuran was stirred and refluxed for 2 hours at reflux temperature. The reaction mixture was filtered while hot over diatomaceous earth and the filtrate was evaporated. The residue was purified by column chromatography over silica gel first using a mixture of trichloromethane and methanol (95:5 by volume) and then a mixture of trichloromethane and methanol, saturated with ammonia, (85:15 by volume) as eluents. The pure fractions were collected and the eluent was evaporated, yielding 50.5 parts (100%) of 5-methoxy-N-(1-methyl-4-piperidinyl)-1H-benzimidazol-2-amine as a residue (interm. 27).

후처리

  1. temperaturerefluxed for 2 hours
  2. temperatureat reflux temperature
  3. filtrationThe reaction mixture was filtered while hot over diatomaceous earth
  4. customthe filtrate was evaporated
  5. customThe residue was purified by column chromatography over silica gel
  6. additiona mixture of trichloromethane and methanol (95:5 by volume)
  7. additiona mixture of trichloromethane and methanol
  8. customThe pure fractions were collected
  9. customthe eluent was evaporated

출처 및 근거

ORD 기록
ord-939f27ad240c45b5b49fdfa90f601f7b
출처 데이터셋
uspto-grants-1990_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04943580

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