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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 21923071, 화합물 → HCID 178478851, 화합물

HRID 1272661
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HRID 1272661 반응식
[NH2:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([NH2:8])[CH2:4][CH2:3]1.[Cl:9][C:10]1[N:18]=[C:17]2[C:13]([N:14]=[CH:15][N:16]2[CH:19]2[CH2:23][CH2:22][CH2:21][CH2:20]2)=[C:12]([NH:24][C:25]2[CH:33]=[CH:32][C:28]([C:29]([NH2:31])=[O:30])=[CH:27][CH:26]=2)[N:11]=1>O>[ClH:9].[ClH:9].[NH2:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([NH:8][C:10]2[N:18]=[C:17]3[C:13]([N:14]=[CH:15][N:16]3[CH:19]3[CH2:20][CH2:21][CH2:22][CH2:23]3)=[C:12]([NH:24][C:25]3[CH:26]=[CH:27][C:28]([C:29]([NH2:31])=[O:30])=[CH:32][CH:33]=3)[N:11]=2)[CH2:4][CH2:3]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 21923071HCID 21923071, 화합물HCID 178511674HCID 178511674, 화합물

생성물 1

HCID 178478851HCID 178478851, 화합물수율 116.9%

시약·촉매·용매 1

HCID 962Water용매

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온도
150 °C

실험 절차

The operation is carried out as in Stage 2 of Example 6 and 800 mg of trans-1,4-diaminocyclohexane is introduced at ambient temperature under agitation then the reaction medium is heated at approximately 150° C. until melting and 249 mg of the product obtained in Stage 1 above is added, the reaction medium is left under agitation for 4 hours 30 minutes then left to return to ambient temperature. Then 10 ml of water is added, followed by extracting with 10 ml of methylene chloride containing 25% of methanol, drying, filtering, evaporating to dryness and taking up in 5 ml of ethanol. 2 ml of 1.4 N HCl in ethanol is added, followed by evaporating, leaving to crystallize, separating and washing with ethanol then drying at a temperature of approximately 60° C. In this way 207 mg of expected product is obtained in the form of colourless crystals.

후처리

  1. additionis introduced at ambient temperature under agitation
  2. waitthen left
  3. customto return to ambient temperature
  4. extractionby extracting with 10 ml of methylene chloride containing 25% of methanol
  5. customdrying
  6. filtrationfiltering
  7. customevaporating to dryness
  8. addition2 ml of 1.4 N HCl in ethanol is added
  9. customby evaporating
  10. customleaving
  11. customto crystallize
  12. customseparating
  13. washwashing with ethanol
  14. customthen drying at a temperature of approximately 60° C

출처 및 근거

ORD 기록
ord-c936872deef543dca63124b424d6f6cd
출처 데이터셋
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07208598B2

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