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

Hydrochloric Acid → Ethyl 2-chloro-3-[4-(6-hydroxy-2,5,7,8-tetramethyl-chroman-2-ylmethoxy)phenyl]propionate

HRID 1589702
ノート
印刷プレビュー

反応式

HRID 1589702 の反応式
C([O:4][C:5]1[C:6]([CH3:34])=[C:7]2[C:12](=[C:13]([CH3:16])[C:14]=1[CH3:15])[O:11][C:10]([CH2:18][O:19][C:20]1[CH:25]=[CH:24][C:23]([CH2:26][CH:27]([Cl:33])[C:28]([O:30][CH2:31][CH3:32])=[O:29])=[CH:22][CH:21]=1)([CH3:17])[CH2:9][CH2:8]2)(=O)C.[O-]CC.[Na+].Cl>C(O)C.O1CCCC1>[Cl:33][CH:27]([CH2:26][C:23]1[CH:22]=[CH:21][C:20]([O:19][CH2:18][C:10]2([CH3:17])[CH2:9][CH2:8][C:7]3[C:12](=[C:13]([CH3:16])[C:14]([CH3:15])=[C:5]([OH:4])[C:6]=3[CH3:34])[O:11]2)=[CH:25][CH:24]=1)[C:28]([O:30][CH2:31][CH3:32])=[O:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 2723922Sodium ethoxideHCID 13605832HCID 13605832、化合物

生成物 1

HCID 20245756Ethyl 2-chloro-3-[4-(6-hydroxy-2,5,7,8-tetramethyl-chroman-2-ylmethoxy)phenyl]propionate

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 8028
Tetrahydrofuran
溶媒

実験手順

0.48 g of ethyl 3-[4-(6-acetoxy-2,5,7,8-tetramethylchroman-2-ylmethoxy)phenyl]-2-chloropropionate was dissolved in a mixture of 3 ml of absolute ethanol and 2 ml of dry tetrahydrofuran. An ethanolic solution of sodium ethoxide (prepared by dissolving 49.0 mg sodium in 2 ml of absolute ethanol) was added dropwise, under a nitrogen stream at 10°-13° C., to the resulting solution. The mixture was then reacted for 21 hours at 0°-5° C., after which 0.22 g of concentrated hydrochloric acid dissolved in 99.5% ethanol was added dropwise, with ice-cooling. The solvent was then distilled off from the reaction mixture under reduced pressure; the separated light reddish oil was extracted with chloroform; and the extract was washed with water and then dried over anhydrous sodium sulfate. The crude product obtained by distilling the chloroform off from the extract under reduced pressure was subjected to silica gel column chromatography, and the desired ethyl 2-chloro-3-[4-(6-hydroxy-2,5,7,8-tetramethyl-chroman-2-ylmethoxy)phenyl]propionate was obtained from the fractions eluted with benzene. Rf value on thin layer chromatography: 0.60 [silica gel; developing solvent; benzene:ethyl acetate=10:1 by volume].

後処理

  1. customThe mixture was then reacted for 21 hours at 0°-5° C.
  2. additionwas added dropwise, with ice-
  3. temperaturecooling
  4. distillationThe solvent was then distilled off from the reaction mixture under reduced pressure
  5. extractionthe separated light reddish oil was extracted with chloroform
  6. washand the extract was washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. customThe crude product obtained
  9. distillationby distilling the chloroform off from the
  10. extractionextract under reduced pressure

出典と根拠

ORDレコード
ord-4161362913cf4a039521453133f3ada1
出典データセット
uspto-grants-1986_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04572912

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