ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

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
ノート
印刷プレビュー

反応式

HRID 2071973 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-570ac7975a4947f38a443fccf0ff7108
出典データセット
uspto-grants-1977_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04049653

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート