Dimethyl acetylenedicarboxylate → HCID 73743288、化合物

HRID 2373514ノート

反応式

HRID 2373514 の反応式
[C:1]([O:5][C:6](=[O:18])[NH:7][C:8]1([C:14]([NH2:17])=[N:15][OH:16])[CH2:13][CH2:12][O:11][CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2].[CH3:19][O:20][C:21]([C:23]#[C:24][C:25]([O:27][CH3:28])=[O:26])=[O:22]>C(Cl)(Cl)Cl>[CH3:19][O:20][C:21](=[O:22])[C:23]([O:16][N:15]=[C:14]([NH2:17])[C:8]1([NH:7][C:6]([O:5][C:1]([CH3:4])([CH3:2])[CH3:3])=[O:18])[CH2:9][CH2:10][O:11][CH2:12][CH2:13]1)=[CH:24][C:25]([O:27][CH3:28])=[O:26]

参加物

4

反応物 2

HCID 12980Dimethyl acetylenedicarboxylateHCID 73743302519031-88-0

生成物 1

HCID 73743288HCID 73743288、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A solution of tert-butyl-4-[amino(hydroxyimino)methyl]tetrahydro-2H-pyran-4-yl-carbamate (C-27) and dimethylacetylendicarboxylate (1.2 eq.) in chloroform was refluxed for 1 hour under nitrogen and the solution was concentrated. Residue was purified bysflash chromatography on silica gel (eluent: petroleum ether:ethyl acetate=7:3) to give the desired product (C-28) as a mixture of isomers in ratio 7:3.

後処理

  1. concentrationthe solution was concentrated
  2. customResidue was purified bysflash chromatography on silica gel (eluent: petroleum ether:ethyl acetate=7:3)

出典と根拠

ORDレコード
ord-ffab033f2d1f4784b714441bc420aa2a
出典データセット
uspto-grants-2008_12
特許番号
US07459452B2

反応ノート

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