Triethylamine → HCID 20031355, 화합물

HRID 232269노트

반응식

HRID 232269 반응식
[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

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 11776TriphenylphosphineHCID 20031357HCID 20031357, 화합물

생성물 1

HCID 20031355HCID 20031355, 화합물

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f2d49f3aa4ca4b60a6cfed005b9a16d4
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04851526

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