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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Dicyclohexylcarbodiimide → 4,4-Dimethyl-7-(4-p-Fluorophenyl-1-Methylbutyl)-9-[4-(Morpholino)-Butyryloxy]-1,2,3,4-Tetrahydrocyclopenta[c] [1]Benzopyran Hydrochloride

HRID 2071973
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HRID 2071973 반응식
[CH3:1][C:2]1([CH3:28])[C:7]2[CH2:8][CH2:9][CH2:10][C:6]=2[C:5]2[C:11]([OH:27])=[CH:12][C:13]([CH:15]([CH3:26])[CH2:16][CH2:17][CH2:18][C:19]3[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=3)=[CH:14][C:4]=2[O:3]1.C1(N=C=NC2CCCCC2)CCCCC1.[ClH:44].[O:45]1[CH2:50][CH2:49][N:48]([CH2:51][CH2:52][CH2:53][C:54](O)=[O:55])[CH2:47][CH2:46]1>C(Cl)Cl>[ClH:44].[CH3:28][C:2]1([CH3:1])[C:7]2[CH2:8][CH2:9][CH2:10][C:6]=2[C:5]2[C:11]([O:27][C:54](=[O:55])[CH2:53][CH2:52][CH2:51][N:48]3[CH2:47][CH2:46][O:45][CH2:50][CH2:49]3)=[CH:12][C:13]([CH:15]([CH3:26])[CH2:16][CH2:17][CH2:18][C:19]3[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=3)=[CH:14][C:4]=2[O:3]1
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참가 물질

5

반응물 3

HCID 10868DicyclohexylcarbodiimideHCID 127337464-Morpholin-4-Yl-Butyric Acid HydrochlorideHCID 214097494,4-Dimethyl-9-hydroxy-7-(4-p-fluorophenyl-1-methylbutyl)-1,2,3,4-tetrahydrocyclopenta [c] [1]benzopyran

생성물 1

HCID 214097584,4-Dimethyl-7-(4-p-Fluorophenyl-1-Methylbutyl)-9-[4-(Morpholino)-Butyryloxy]-1,2,3,4-Tetrahydrocyclopenta[c] [1]Benzopyran Hydrochloride

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

7.10 g. (18.7 mmoles) of 4,4-dimethyl-9-hydroxy-7-(4-p-fluorophenyl-1-methylbutyl)-1,2,3,4-tetrahydrocyclopenta [c] [1]benzopyran, prepared according to the method of Example 6, 4.33 g. (21.0 mmoles) of dicyclohexylcarbodiimide and 4.26 g. (20.3 mmoles) of γ-morpholinobutyric acid hydrochloride are combined with 325 ml. of methylene chloride and stirred at room temperature for a total of 24 hours. The insoluble by-product of dicyclohexylurea is separated by filtration and the methylene chloride is removed using a rotary evaporator. The viscous residue is dissolved in about 100 ml. of benzene and the benzene solution is filtered to remove a small amount of insoluble material. The benzene is removed using a rotary evaporator and the remaining residue is triturated with approximately 250 ml. of ether. The solid which forms is filtered, washed with ether and dried to yield a solid. The material is crystallized from benzene/ether to give the solid product.

후처리

  1. customThe insoluble by-product of dicyclohexylurea is separated by filtration
  2. customthe methylene chloride is removed
  3. customa rotary evaporator
  4. dissolutionThe viscous residue is dissolved in about 100 ml
  5. filtrationof benzene and the benzene solution is filtered
  6. customto remove a small amount of insoluble material
  7. customThe benzene is removed
  8. customa rotary evaporator
  9. customthe remaining residue is triturated with approximately 250 ml
  10. filtrationThe solid which forms is filtered
  11. washwashed with ether
  12. customdried
  13. customto yield a solid
  14. customThe material is crystallized from benzene/ether
  15. customto give the solid product

출처 및 근거

ORD 기록
ord-570ac7975a4947f38a443fccf0ff7108
출처 데이터셋
uspto-grants-1977_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04049653

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