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 → 1-[4-(Thiomorpholino)butyryloxy]-3-(3-methyl-2-octyl)-6,6,9-trimethyl-7,8,9,10-tetrahydro-6H-dibenzo[b,d] pyran

HRID 267351
ノート
印刷プレビュー

反応式

HRID 267351 の反応式
[OH:1][C:2]1[C:11]2[C:10]3[CH2:12][CH:13]([CH3:16])[CH2:14][CH2:15][C:9]=3[C:8]([CH3:18])([CH3:17])[O:7][C:6]=2[CH:5]=[C:4]([CH:19]([CH:21]([CH3:27])[CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])[CH3:20])[CH:3]=1.Cl.[S:29]1[CH2:34][CH2:33][N:32]([CH2:35][CH2:36][CH2:37][C:38](O)=[O:39])[CH2:31][CH2:30]1.C1(N=C=NC2CCCCC2)CCCCC1>C(Cl)Cl>[S:29]1[CH2:30][CH2:31][N:32]([CH2:35][CH2:36][CH2:37][C:38]([O:1][C:2]2[C:11]3[C:10]4[CH2:12][CH:13]([CH3:16])[CH2:14][CH2:15][C:9]=4[C:8]([CH3:17])([CH3:18])[O:7][C:6]=3[CH:5]=[C:4]([CH:19]([CH:21]([CH3:27])[CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])[CH3:20])[CH:3]=2)=[O:39])[CH2:33][CH2:34]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 362763-(1,2-dimethylheptyl)-7,8,9,10-tetrahydro-6,6,9-trimethyl-6H-dibenzo(b,d)pyran-1-olHCID 70633382gamma-Thiomorpholinobutyric acid hydrochloride

生成物 1

HCID 537268201-[4-(Thiomorpholino)butyryloxy]-3-(3-methyl-2-octyl)-6,6,9-trimethyl-7,8,9,10-tetrahydro-6H-dibenzo[b,d] pyran

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

A mixture of 4.0 g. (10.8 mmole) of 1-hydroxy-3-(3-methyl-2-octyl)-6,6,9-trimethyl-7,8,9,10-tetrahydro-6H-dibenzo[ b,d] pyran, 2.4 g. (10.8 mmole) of γ-thiomorpholinobutyric acid hydrochloride, 2.38 g. (11.5 mmole) of dicyclohexylcarbodiimide and 250 ml. of methylene chloride was stirred and heated at reflux for 18 hours. After cooling the reaction mixture, the byproduct of dicyclohexylurea was removed by suction filtration. The solvent was evaporated to give a red-brown residue which was chromatographed using 90 g. of activated magnesium silicate (60-100 mesh) and chloroform as the solvent system. The fractions were monitored by thin layer chromatography, and the appropriate fractions were combined and evaporated to give 1.0 g. of a light yellow oil. The material was pure by thin layer chromatography, and the infrared and nuclear magnetic resonance spectra were in agreement with the designated structure.

後処理

  1. additionA mixture of 4.0 g
  2. temperatureheated
  3. temperatureat reflux for 18 hours
  4. temperatureAfter cooling the reaction mixture
  5. customthe byproduct of dicyclohexylurea was removed by suction filtration
  6. customThe solvent was evaporated
  7. customto give a red-brown residue which
  8. customwas chromatographed
  9. customevaporated
  10. customto give 1.0 g

出典と根拠

ORDレコード
ord-1d42ce80a6b4417581a7d0d82cf085a4
出典データセット
uspto-grants-1976_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03941782

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