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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 21923073, 화합물 → HCID 178478728, 화합물

HRID 1244950
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HRID 1244950 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:30]=[CH:29][C:28]([C:31]([F:34])([F:33])[F:32])=[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:30]=[CH:29][C:28]([C:31]([F:32])([F:34])[F:33])=[CH:27][CH:26]=3)[N:11]=2)[CH2:4][CH2:3]1
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참가 물질

4

반응물 2

HCID 21923073HCID 21923073, 화합물HCID 178511674HCID 178511674, 화합물

생성물 1

HCID 178478728HCID 178478728, 화합물

시약·촉매·용매 1

HCID 962Water용매

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온도
140 °C

실험 절차

684 mg of trans-1,4-diaminocyclohexane is taken to approximately 150° C. then 229 mg of the product obtained in Stage 1 above is added, the reaction medium is maintained under agitation at 140° C. for 5 hours then left to return to ambient temperature. Then 15 ml of water is added, followed by extracting with dichloromethane, drying and evaporating the solvent. The residue is chromatographed on silica (eluent: MeOH/NH4OH 98/2), taken up in 10 ml of ethanol, 6 ml of an ethanolic solution of hydrochloric acid is added, followed by separating, washing with ether, drying under reduced pressure at 60° C. and 159 mg of expected product is recovered.

후처리

  1. customis taken to approximately 150° C.
  2. waitthen left
  3. customto return to ambient temperature
  4. extractionby extracting with dichloromethane
  5. customdrying
  6. customevaporating the solvent
  7. customThe residue is chromatographed on silica (eluent: MeOH/NH4OH 98/2)
  8. addition6 ml of an ethanolic solution of hydrochloric acid is added
  9. customby separating
  10. washwashing with ether
  11. customdrying under reduced pressure at 60° C.
  12. custom159 mg of expected product is recovered

출처 및 근거

ORD 기록
ord-5250a7a6082a492188cc1a56b1273e96
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07122669B1

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