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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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3-(N-methylsulfonyl-N-tert-butoxycarbonylamino)-4-benzyloxy-1-(2,3-epoxypropoxy)-benzene → 1-(3-Methylsulfonylamino-4-benzyloxyphenoxy)-3-(7-piperidinocarbonylmethoxy-tetralin-2-yl-amino)-2-propanol

HRID 1796417
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HRID 1796417 반응식
[CH3:1][S:2]([N:5]([C:13]1[CH:14]=[C:15]([O:27][CH2:28][CH:29]2[O:31][CH2:30]2)[CH:16]=[CH:17][C:18]=1[O:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)C(OC(C)(C)C)=O)(=[O:4])=[O:3].[NH2:32][CH:33]1[CH2:42][CH2:41][C:40]2[C:35](=[CH:36][C:37]([O:43][CH2:44][C:45]([N:47]3[CH2:52][CH2:51][CH2:50][CH2:49][CH2:48]3)=[O:46])=[CH:38][CH:39]=2)[CH2:34]1>C(O)C>[CH3:1][S:2]([NH:5][C:13]1[CH:14]=[C:15]([CH:16]=[CH:17][C:18]=1[O:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[O:27][CH2:28][CH:29]([OH:31])[CH2:30][NH:32][CH:33]1[CH2:42][CH2:41][C:40]2[C:35](=[CH:36][C:37]([O:43][CH2:44][C:45]([N:47]3[CH2:52][CH2:51][CH2:50][CH2:49][CH2:48]3)=[O:46])=[CH:38][CH:39]=2)[CH2:34]1)(=[O:4])=[O:3]
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참가 물질

4

반응물 2

HCID 114650773-(N-methylsulfonyl-N-tert-butoxycarbonylamino)-4-benzyloxy-1-(2,3-epoxypropoxy)-benzeneHCID 155116422-Amino-7-piperidinocarbonylmethoxy-tetralin

생성물 1

HCID 221820811-(3-Methylsulfonylamino-4-benzyloxyphenoxy)-3-(7-piperidinocarbonylmethoxy-tetralin-2-yl-amino)-2-propanol수율 39.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2.34 g (0.0052 mole) of 3-(N-methylsulfonyl-N-tert-butoxycarbonylamino)-4-benzyloxy-1-(2,3-epoxypropoxy)-benzene, 71 ml of ethanol and 1.44 g (0.0052 mole) of 2-amino-7-piperidinocarbonylmethoxy-tetralin from preparation 1 (base, racemate) were heated under reflux for 8 hours. It was stirred at ambient temperature overnight and then it was heated again under reflux for a further 6 hours. The solvent was evaporated off, the residue was taken up in 40 ml of ethyl acetate and 32.1 ml of a 3N solution of hydrochloric acid in ethyl acetate were added. It was heated under reflux for 5 hours and evaporated under reduced pressure. It was taken up in water, NH4OH was added until the pH was basic, and it was extracted with ethyl acetate. It was dried, the solvent was evaporated off and the product was purified by silica gel column flash chromatography, eluting with a 9:1 methylene chloride/methanol mixture. 1.3 g of the product of the heading was obtained.

후처리

  1. temperaturewere heated
  2. temperatureunder reflux for 8 hours
  3. temperatureit was heated again
  4. temperatureunder reflux for a further 6 hours
  5. customThe solvent was evaporated off
  6. addition32.1 ml of a 3N solution of hydrochloric acid in ethyl acetate were added
  7. temperatureIt was heated
  8. temperatureunder reflux for 5 hours
  9. customevaporated under reduced pressure
  10. additionNH4OH was added until the pH
  11. extractionit was extracted with ethyl acetate
  12. customIt was dried
  13. customthe solvent was evaporated off
  14. customthe product was purified by silica gel column flash chromatography
  15. washeluting with a 9:1 methylene chloride/methanol mixture

출처 및 근거

ORD 기록
ord-a0c38d44d04e42ae816b498f7cf4c7ea
출처 데이터셋
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07030160B2

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