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

Diisopropylamine → HCID 59570922、化合物

HRID 2192905
ノート
印刷プレビュー

反応式

HRID 2192905 の反応式
C(NC(C)C)(C)C.C([Li])CCC.CCCCCC.[Br:19][C:20]1[CH:21]=[C:22]([CH2:32][C:33]([O:35][CH3:36])=[O:34])[CH:23]=[CH:24][C:25]=1[S:26]([CH:29]1[CH2:31][CH2:30]1)(=[O:28])=[O:27].I[CH2:38][C@H:39]1[CH2:59][CH2:58][C:41]2([O:45][C@H:44]([C:46]3[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=3)[C@@H:43]([C:52]3[CH:57]=[CH:56][CH:55]=[CH:54][CH:53]=3)[O:42]2)[CH2:40]1>C1COCC1.O.CN1CCCN(C)C1=O>[Br:19][C:20]1[CH:21]=[C:22]([CH:32]([CH2:38][C@H:39]2[CH2:59][CH2:58][C:41]3([O:45][C@H:44]([C:46]4[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=4)[C@@H:43]([C:52]4[CH:57]=[CH:56][CH:55]=[CH:54][CH:53]=4)[O:42]3)[CH2:40]2)[C:33]([O:35][CH3:36])=[O:34])[CH:23]=[CH:24][C:25]=1[S:26]([CH:29]1[CH2:31][CH2:30]1)(=[O:28])=[O:27]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 7912DiisopropylamineHCID 21051867(2R,3R,7S)-7-(iodomethyl)-2,3-diphenyl-1,4-dioxaspiro[4.4]nonaneHCID 59570968HCID 59570968、化合物HCID 178418244HCID 178418244、化合物

生成物 1

HCID 59570922HCID 59570922、化合物収率 72.4%

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 8028Tetrahydrofuran溶媒4 回
HCID 816462(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl-溶媒2 回

反応条件

温度
-50 °C

実験手順

To a mixture of diisopropylamine (6.94 mL), 1,3-dimethyltetrahydropyrimidin-2(1H)-one (18 mL) and THF (60 mL) was added 2.64 M n-butyl lithium/hexane solution (18.4 mL) at an internal temperature of −50° C. or lower, followed by stirring at an internal temperature of −50° C. or lower for 1 hour. To the reaction mixture was added dropwise a solution of methyl [3-bromo-4-(cyclopropylsulfonyl)phenyl]acetate (15.0 g) in THF (20 mL)/1,3-dimethyl tetrahydropyrimidin-2(1H)-one (9 mL) at an internal temperature of −50° C. or lower, followed by stirring at the same temperature for 30 minutes, and THF (30 mL) was added thereto, followed by stirring at −20° C. for 1 hour. A solution of (2R,3R,7S)-7-(iodomethyl)-2,3-diphenyl-1,4-dioxaspiro[4.4]nonane (21.8 g) in THF (20 mL) was added dropwise thereto at an internal temperature of −60° C. or lower, followed by stirring at the same temperature for 30 minutes and then stirring at room temperature overnight. To the reaction mixture was added water (200 mL) under ice-cooling, followed by extraction with ethyl acetate (100 mL×3). The organic layer was sequentially washed with water (200 mL) and saturated brine (200 mL), and dried over anhydrous magnesium sulfate, and the solvent was then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate 19:1→1:1) to obtain methyl 2-[3-bromo-4-(cyclopropylsulfonyl)phenyl]-3-[(2R,3R,7R)-2,3-diphenyl-1,4-dioxaspiro[4.4]non-7-yl]propionate (20.4 g) as a pale yellow amorphous substance.

後処理

  1. stirringby stirring at the same temperature for 30 minutes
  2. stirringby stirring at −20° C. for 1 hour
  3. customat an internal temperature of −60° C.
  4. stirringby stirring at the same temperature for 30 minutes
  5. stirringstirring at room temperature overnight
  6. temperaturecooling
  7. extractionfollowed by extraction with ethyl acetate (100 mL×3)
  8. washThe organic layer was sequentially washed with water (200 mL) and saturated brine (200 mL)
  9. dry with materialdried over anhydrous magnesium sulfate
  10. customthe solvent was then evaporated under reduced pressure
  11. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate 19:1→1:1)

出典と根拠

ORDレコード
ord-e55b5d05d6a84117b7cdb1da02edc2c4
出典データセット
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08329707B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート