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Methyl 3-mercaptopropionate → Methyl 3-[(5,6-dimethoxypyridin-3-yl)sulfanyl]propanoate

HRID 709022
ノート
印刷プレビュー

反応式

HRID 709022 の反応式
Br[C:2]1[CH:3]=[C:4]([O:10][CH3:11])[C:5]([O:8][CH3:9])=[N:6][CH:7]=1.[SH:12][CH2:13][CH2:14][C:15]([O:17][CH3:18])=[O:16].C(N(C(C)C)C(C)C)C>O1CCOCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2>[CH3:11][O:10][C:4]1[CH:3]=[C:2]([S:12][CH2:13][CH2:14][C:15]([O:17][CH3:18])=[O:16])[CH:7]=[N:6][C:5]=1[O:8][CH3:9]
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 3

HCID 18050Methyl 3-mercaptopropionateHCID 81531DiisopropylethylamineHCID 125630845-Bromo-2,3-dimethoxypyridine

生成物 1

HCID 71185962Methyl 3-[(5,6-dimethoxypyridin-3-yl)sulfanyl]propanoate収率 105.1%

試薬・触媒・溶媒 3

HCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)触媒
HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 312751,4-Dioxane溶媒

実験手順

To a solution of 5-bromo-2,3-dimethoxypyridine (2 g, 9.17 mmol) in dioxane (30 ml) was added methyl 3-sulfanylpropanoate (1.21 g, 10.1 mmol), N-ethyl-N-isopropylpropan-2-amine (3.03 ml, 18.3 mmol), Pd2(dba)3 (0.34 g, 0.37 mmol) and Xantphos (0.43 g, 0.73 mmol) at room temperature under an atmosphere of nitrogen. The reaction was degassed by evacuating and flushing with nitrogen and heated at reflux for 18 hours and then allowed to cool and filtered, washing with ethyl acetate. The filtrate was concentrated under reduced pressure to give an orange oil. Purification by column chromatography (SiO2; 0-20% ethyl acetate in petrol), gave methyl 3-[(5,6-dimethoxypyridin-3-yl)sulfanyl]propanoate as a yellow oil (2.48 g, quantitative yield).

後処理

  1. customThe reaction was degassed
  2. customby evacuating
  3. customflushing with nitrogen
  4. temperatureheated
  5. temperatureat reflux for 18 hours
  6. temperatureto cool
  7. filtrationfiltered
  8. washwashing with ethyl acetate
  9. concentrationThe filtrate was concentrated under reduced pressure
  10. customto give an orange oil
  11. customPurification by column chromatography (SiO2; 0-20% ethyl acetate in petrol)

出典と根拠

ORDレコード
ord-3605c11a11c6418797d31b2d9e413b93
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09180122B2

反応ノート

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