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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
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Water → HCID 68110364、化合物

HRID 1752485
ノート
印刷プレビュー

反応式

HRID 1752485 の反応式
[CH3:1][O:2][C:3]([C:5]1[C:10]([NH2:11])=[N:9][C:8](Cl)=[CH:7][N:6]=1)=[O:4].[CH2:13]([Sn](CCCC)(CCCC)C=C)[CH2:14]CC.[Cl-].[Li+].O>CN(C=O)C.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[CH3:1][O:2][C:3]([C:5]1[C:10]([NH2:11])=[N:9][C:8]([CH:13]=[CH2:14])=[CH:7][N:6]=1)=[O:4]
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

7

反応物 4

HCID 962WaterHCID 81998TributylvinyltinHCID 433294Lithium ChlorideHCID 53417426Methyl 3-amino-5-chloropyrazine-2-carboxylate

生成物 1

HCID 68110364HCID 68110364、化合物

試薬・触媒・溶媒 2

HCID 178418476HCID 178418476、化合物触媒
HCID 6228
Dimethylformamide
溶媒

反応条件

温度
85 °C

実験手順

To a mixture of 3-amino-5-chloro-pyrazine-2-carboxylic acid methyl ester (GB 1248146, 161 mg 0.86 mmol), tributyl(vinyl)tin (0.352 ml, 1.204 mmol) and lithium chloride (102 mg, 2.498 mmol) in DMF (4 ml) was added PdCl2(PPh3)2 (30.2 mg, 0.043 mmol) and the mixture was heated to 85° C. for 2.5 h. After cooling to room temperature water was added and the mixture was extracted with EtOAc, the combined organic layers were washed with water and half saturated aq. NaCl, dried with Na2SO4 and evaporated. The residue was purified by chromatography on silica gel (cyclohexane to cyclohexane/EtOAc 1:9) to provide the title compound as yellow solid.

後処理

  1. additionwas added
  2. extractionthe mixture was extracted with EtOAc
  3. washthe combined organic layers were washed with water and half saturated aq. NaCl
  4. dry with materialdried with Na2SO4
  5. customevaporated
  6. customThe residue was purified by chromatography on silica gel (cyclohexane to cyclohexane/EtOAc 1:9)

出典と根拠

ORDレコード
ord-5d0db4964ef7432bb2f515f7c8c08628
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09163011B2

反応ノート

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