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Water → HCID 67397694、化合物

HRID 70655
ノート
印刷プレビュー

反応式

HRID 70655 の反応式
C([SnH](CCCC)CCCC)CCC.N(C(C)(C)C#N)=NC(C)(C)C#N.C(SC)(=S)O[CH:28]([C:30]1[C:31]([O:65][CH3:66])=[N:32][C:33](/[C:36](/[C:55]2[CH:60]=[CH:59][C:58]([C:61]([CH3:64])([CH3:63])[CH3:62])=[CH:57][CH:56]=2)=[CH:37]/[C@H:38]2[CH2:42][CH2:41][C:40](=[O:43])[N:39]2[CH2:44][C:45]2[CH:50]=[CH:49][C:48]([O:51][CH3:52])=[CH:47][C:46]=2[O:53][CH3:54])=[CH:34][CH:35]=1)[CH3:29].O>C1(C)C=CC=CC=1>[C:61]([C:58]1[CH:59]=[CH:60][C:55](/[C:36](/[C:33]2[CH:34]=[CH:35][C:30]([CH2:28][CH3:29])=[C:31]([O:65][CH3:66])[N:32]=2)=[CH:37]\[C@@H:38]2[N:39]([CH2:44][C:45]3[CH:50]=[CH:49][C:48]([O:51][CH3:52])=[CH:47][C:46]=3[O:53][CH3:54])[C:40](=[O:43])[CH2:41][CH2:42]2)=[CH:56][CH:57]=1)([CH3:63])([CH3:62])[CH3:64]
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

6

反応物 4

HCID 962WaterHCID 5948TributylstannaneHCID 6547AzobisisobutyronitrileHCID 86658011HCID 86658011、化合物

生成物 1

HCID 67397694HCID 67397694、化合物収率 71.6%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
120 °C

実験手順

Tributyltin hydride (91 μL) and azobisisobutyronitrile (8.5 mg) were added to a solution of O-[1-(6-{(E)-1-(4-tert-butylphenyl)-2-[(2R)-1-(2,4-dimethoxybenzyl)-5-oxopyrrolidin-2-yl]ethenyl}-2-methoxypyridin-3-yl)ethyl] S-methyl carbonodithioate (109 mg) in toluene (2 mL), and the mixture was stirred at 120° C. for 30 minutes. Water was added to the reaction solution, followed by extraction with chloroform. The organic layer was dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1) to give (5R)-5-[(E)-2-(4-tert-butylphenyl)-2-(5-ethyl-6-methoxypyridin-2-yl)ethenyl]-1-(2,4-dimethoxybenzyl)pyrrolidin-2-one as a colorless oil (65 mg).

後処理

  1. extractionfollowed by extraction with chloroform
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. customThe solvent was then evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1)

出典と根拠

ORDレコード
ord-86061efff23f4881bc33545b3bf7e433
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822503B2

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