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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
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trans-1,2-Diacetoxy-1,2-dihydrobenzocyclobutene → Methyl rac-1',2',3',4',5',5a',6',11',11a',12'-decahydro-6',11'-diacetoxy-5',12'-dioxospiro[1,3-dithiolane-2,4'-naphthacene]-2'-carboxylate

HRID 463467
ノート
印刷プレビュー

反応式

HRID 463467 の反応式
[C:1]([O:4][C@@H:5]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[C@H:6]1[O:13][C:14](=[O:16])[CH3:15])(=[O:3])[CH3:2].[O:17]=[C:18]1[CH:27]=[CH:26][C:25](=[O:28])[C:24]2[CH2:23][CH:22]([C:29]([O:31][CH3:32])=[O:30])[CH2:21][C:20]3([S:36][CH2:35][CH2:34][S:33]3)[C:19]1=2>C1(C)C(C)=CC=CC=1>[C:14]([O:13][CH:6]1[C:7]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH:5]([O:4][C:1](=[O:3])[CH3:2])[CH:26]2[CH:27]1[C:18](=[O:17])[C:19]1[C:20]3([S:36][CH2:35][CH2:34][S:33]3)[CH2:21][CH:22]([C:29]([O:31][CH3:32])=[O:30])[CH2:23][C:24]=1[C:25]2=[O:28])(=[O:16])[CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 13264175trans-1,2-Diacetoxy-1,2-dihydrobenzocyclobuteneHCID 20283295Methyl rac-1',2',3',4',5',8'-hexahydro-5',8'-dioxospiro[1,3-dithiolane-2,4'-naphthalene]-2'-carboxylate

生成物 1

HCID 20283276Methyl rac-1',2',3',4',5',5a',6',11',11a',12'-decahydro-6',11'-diacetoxy-5',12'-dioxospiro[1,3-dithiolane-2,4'-naphthacene]-2'-carboxylate収率 62%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

A solution of 0.757 g (3.4 mmol) of trans-1,2-diacetoxy-1,2-dihydrobenzocyclobutene and 0.970 g (3.1 mmol) of methyl rac-1',2',3',4',5',8'-hexahydro-5',8'-dioxospiro[1,3-dithiolane-2,4'-naphthalene]-2'-carboxylate [prepared as described in Example 2(A)] in 100 ml of dry xylene was stirred and heated under reflux under an atmosphere of nitrogen for 1 hour. The mixture was evaporated to dryness and the resulting brown oil was triturated with 10 ml of diethyl ether, cooled and filtered to give 1.02 g (61.5%) of methyl rac-1',2',3',4',5',5a',6',11',11a',12'-decahydro-6',11'-diacetoxy-5',12'-dioxospiro[1,3-dithiolane-2,4'-naphthacene]-2'-carboxylate in the form of a pale yellow solid of melting point 174°-175° C.

後処理

  1. temperatureheated
  2. temperatureunder reflux under an atmosphere of nitrogen for 1 hour
  3. customThe mixture was evaporated to dryness
  4. customthe resulting brown oil was triturated with 10 ml of diethyl ether
  5. temperaturecooled
  6. filtrationfiltered

出典と根拠

ORDレコード
ord-7f744563c4854fc78e9e6bf31ef97bce
出典データセット
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04518784

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