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Ethanol → HCID 86614568、化合物

HRID 1766089
ノート
印刷プレビュー

反応式

HRID 1766089 の反応式
C(=O)([O-])[O-].[K+].[K+].[CH2:7]([CH:9]([C:17]([O-:19])=[O:18])[C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH3:8].[C:20]([C:22]1[C:23]([C:32]2[CH:37]=[CH:36][CH:35]=[C:34]([N+:38]([O-:40])=[O:39])[CH:33]=2)=[N:24][C:25]([S:30][CH3:31])=[N:26][C:27]=1C=C)#[N:21].[CH3:41][CH2:42]O>C1(C)C=CC=CC=1.C(Cl)Cl.CCOC(C)=O>[C:20]([C:22]1[C:23]([C:32]2[CH:37]=[CH:36][CH:35]=[C:34]([N+:38]([O-:40])=[O:39])[CH:33]=2)=[N:24][C:25]([S:30][CH3:31])=[N:26][C:27]=1[CH2:8][CH2:7][CH:9]([C:17]([O:19][CH2:41][CH3:42])=[O:18])[C:10]([O:12][C:13]([CH3:15])([CH3:14])[CH3:16])=[O:11])#[N:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 702EthanolHCID 11430Potassium CarbonateHCID 21109084HCID 21109084、化合物HCID 85608643HCID 85608643、化合物

生成物 1

HCID 86614568HCID 86614568、化合物

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒
HCID 21877217
Toluene methylene chloride
溶媒

実験手順

Potassium carbonate (1.88 g) and tert-butyl ethylmalonate were suspended in EtOH (82 ml) and a solution of 5-cyano-2-methylthio-4-(3-nitro-phenyl)-6-vinylpyrimidine (example 27b, 2.71 g) in toluene/CH2Cl2 (33 ml) was slowly added (ca 1.5 h). After the addition was complete, the mixture was stirred for an additional 40 min. The mixture was diluted with EtOAc and washed with water (2×) and brine. The organic layer was dried (MgSO4) and concentrated under reduced pressure. The title compound was purified by chromatography on silica gel with hept/CH2Cl2=1/1 (v/v) as eluent.

後処理

  1. additionAfter the addition
  2. washwashed with water (2×) and brine
  3. dry with materialThe organic layer was dried (MgSO4)
  4. concentrationconcentrated under reduced pressure
  5. customThe title compound was purified by chromatography on silica gel with hept/CH2Cl2=1/1 (v/v) as eluent

出典と根拠

ORDレコード
ord-9bf84ca3af0c4590b086e1e7c126b7e8
出典データセット
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07229990B2

反応ノート

読み込み中…

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