Triethylamine → HCID 20031355、化合物

HRID 232269ノート

反応式

HRID 232269 の反応式
[CH:1]1([CH2:7][NH:8][CH2:9][CH:10]([CH2:13][OH:14])[CH2:11]O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(N(CC)CC)C>C(Cl)(Cl)(Cl)Cl>[CH:1]1([CH2:7][N:8]2[CH2:9][CH:10]([CH2:13][OH:14])[CH2:11]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 11776TriphenylphosphineHCID 20031357HCID 20031357、化合物

生成物 1

HCID 20031355HCID 20031355、化合物

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

To 100 mL of carbon tetrachloride add 19.2 g (0.1 mol) of 2-[(cyclohexylmethylamino)methyl]-1,3-propanediol, 26.2 g (0.1 mol) of triphenylphosphine, and 11 g (0.1 mol) of triethylamine. Monitor the reaction by thin-layer chromatography. Upon completion extract twice with 50 mL of 1N aqueous HCl. Add 1N NaOH to the aqueous portion until basic and extract twice with 100 mL of ether. Dry the organic phase over Na2SO4. Filter off the drying agent and evaporate the solvent in vacuo to obtain the title compound.

後処理

  1. customMonitor the reaction by thin-layer chromatography
  2. extractionUpon completion extract twice with 50 mL of 1N aqueous HCl
  3. additionAdd 1N NaOH to the aqueous portion until basic and
  4. extractionextract twice with 100 mL of ether
  5. dry with materialDry the organic phase over Na2SO4
  6. filtrationFilter off the drying agent
  7. customevaporate the solvent in vacuo

出典と根拠

ORDレコード
ord-f2d49f3aa4ca4b60a6cfed005b9a16d4
出典データセット
uspto-grants-1989_07
特許番号
US04851526

反応ノート

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