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Dimethylamine → HCID 57210056、化合物

HRID 1976365
ノート
印刷プレビュー

反応式

HRID 1976365 の反応式
[CH3:1][NH:2][CH3:3].ClCCl.[CH3:7][O:8][C:9]([C:11]1[C@H:12]2[CH2:29][C@@H:28]3[O:30][C@:27]3(C)[C@@H:13]2[C@H:14]([O:17][C:18](OC2C=CC=CC=2)=[O:19])[O:15][CH:16]=1)=[O:10]>CCCCCC.C(OCC)(=O)C>[CH3:7][O:8][C:9]([C:11]1[C@H:12]2[CH2:29][C@@H:28]3[O:30][C@@H:27]3[C@@H:13]2[C@H:14]([O:17][C:18](=[O:19])[N:2]([CH3:3])[CH3:1])[O:15][CH:16]=1)=[O:10]
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 674DimethylamineHCID 6344DichloromethaneHCID 57009109HCID 57009109、化合物

生成物 1

HCID 57210056HCID 57210056、化合物収率 83%

試薬・触媒・溶媒 1

HCID 21226206Ethyl acetate hexane溶媒

実験手順

5 ml of a 50% aqueous dimethylamine solution were added to a dichloromethane solution containing 198 mg of (1S,4aS,6S,7R,7aR)-6,7-epoxy-1,4a,5,6,7,7a-hexahydro-7-methyl-1-(phenoxycarbonyloxy) cyclopenta [c] pyrane-4-carboxylic acid methylester described in Example 10 followed by stirring for 10 minutes at room temperature. The reaction mixture was then extracted with dichloromethane. After washing the organic phase with brine, it was dried over anhydrous magnesium sulfate. After distilling off the solvent under reduced pressure, the residue was purified by silica gel chromatography to obtain a colorless powder from the hexane-ethyl acetate eluate in the form of (1S,4aS,6S,7R,7aR)-1-(dimethylcarbamoyloxy)-6,7-epoxy-1,4a,5,6,7,7a-hexahydrocyclopenta [c] pyrane-4-carboxylic acid methylester (140 mg, yield: 83%). The physicochemical properties of this compound are described in Table 7. Compound No. 31.

後処理

  1. extractionThe reaction mixture was then extracted with dichloromethane
  2. washAfter washing the organic phase with brine, it
  3. dry with materialwas dried over anhydrous magnesium sulfate
  4. distillationAfter distilling off the solvent under reduced pressure
  5. customthe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-b0b2f7ad60f14f5289444ed1724a734e
出典データセット
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06225478B1

反応ノート

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