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Formaldehyde → 1-Diethylamino-6-(3,4-dimethoxyphenyl)hex-2-yne

HRID 1414941
ノート
印刷プレビュー

反応式

HRID 1414941 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][CH2:13][C:14]#[CH:15])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].O1[CH2:21][CH2:20]COO1.C=O.[CH2:24]([NH:26][CH2:27]C)[CH3:25].[OH-].[Na+]>O1CCOCC1.C(O)(=O)C.O>[CH2:24]([N:26]([CH2:20][CH3:21])[CH2:27][C:15]#[C:14][CH2:13][CH2:12][CH2:11][C:5]1[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=1)[CH3:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 712FormaldehydeHCID 8021DiethylamineHCID 14798Sodium HydroxideHCID 19593658CID 19593658HCID 214858375-(3,4-Dimethoxyphenyl)-pent-1-yne

生成物 1

HCID 214857251-Diethylamino-6-(3,4-dimethoxyphenyl)hex-2-yne

試薬・触媒・溶媒 3

HCID 176
Acetic Acid
溶媒
HCID 962Water溶媒
HCID 312751,4-Dioxane溶媒

実験手順

Heat a mixture of 5-(3,4-dimethoxyphenyl)-pent-1-yne (8 g), water (2.5 cc), trioxan (0.5 g ), 30% formalin (5.5 g), diethylamine (4 g), acetic acid (2.75 g), dioxan (25 cc) and cuprous chloride (0.13 g) at 70° for 15 hours. Make the cooled solution alkaline with 10% aqueous sodium hydroxide and collect the product. Wash the ethereal solution with water and extract with 10% hydrochloric acid (3 × 30 cc). Wash the combined aqueous extracts with ether, make it alkaline with 10% sodium hydroxide solution and extract with ether. Wash and dry the ethereal solution, evaporate the solvent and distil the residue at 0.1 mm Hg to obtain 1-diethylamino-6-(3,4-dimethoxyphenyl)-hex-2-yne.

後処理

  1. temperatureHeat
  2. customcollect the product
  3. washWash the ethereal solution with water
  4. extractionextract with 10% hydrochloric acid (3 × 30 cc)
  5. washWash the combined aqueous extracts with ether
  6. extractionextract with ether
  7. washWash
  8. customdry the ethereal solution
  9. customevaporate the solvent
  10. customdistil the residue at 0.1 mm Hg

出典と根拠

ORDレコード
ord-48bbbec8e91840ae901612f74f490c37
出典データセット
uspto-grants-1977_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04002746

反応ノート

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