Water → 2-(Triphenylmethoxy)ethan-1-amine

HRID 80300

반응식

HRID 80300 반응식
[C:1]1([C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)Cl)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.[CH2:22]([CH2:24][NH2:25])[OH:23].O>N1C=CC=CC=1>[C:1]1([C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[O:23][CH2:22][CH2:24][NH2:25])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 6456Trityl chlorideHCID 74819Ethanolamine Hydrochloride

생성물 1

HCID 138305502-(Triphenylmethoxy)ethan-1-amine수율 28.5%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

Triphenylchloromethane (1.00 g, 3.58 mmol) (Wako Pure Chemical Industries, Ltd.) and ethanolamine hydrochloride (1.00 g, 10.3 mmol) (Wako Pure Chemical Industries, Ltd.) were dissolved in pyridine (4 mL), and the solution was stirred at room temperature for 3 days. Water (200 mL) was poured into the reaction solution, and the precipitates were suction-filtered. The solid matters were suspended in diethyl ether, and 3 (N) hydrochloric acid (Wako Pure Chemical Industries, Ltd.) was added thereto, followed by stirring at room temperature for 15 minutes. The insoluble matters were suction-filtered. The insoluble matters were dissolved in a mixed solution of ethyl acetate (Wako Pure Chemical Industries, Ltd.) and a saturated aqueous solution of sodium hydrogen carbonate (Wako Pure Chemical Industries, Ltd.), and the mixture was shaken, followed by the separation of the organic layer. The organic layer was dried with anhydrous sodium sulfate (Wako Pure Chemical Industries, Ltd.), and then suction-filtered and concentrated under reduced pressure, to thereby obtain the title compound (0.31 g, 28% yield).

후처리

  1. filtrationthe precipitates were suction-filtered
  2. addition3 (N) hydrochloric acid (Wako Pure Chemical Industries, Ltd.) was added
  3. stirringby stirring at room temperature for 15 minutes
  4. filtrationThe insoluble matters were suction-filtered
  5. dissolutionThe insoluble matters were dissolved in a mixed solution of ethyl acetate (Wako Pure Chemical Industries, Ltd.)
  6. stirringa saturated aqueous solution of sodium hydrogen carbonate (Wako Pure Chemical Industries, Ltd.), and the mixture was shaken
  7. customfollowed by the separation of the organic layer
  8. dry with materialThe organic layer was dried with anhydrous sodium sulfate (Wako Pure Chemical Industries, Ltd.)
  9. filtrationsuction-filtered
  10. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-ecd98778443d418ba5795531736883e0
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846012B2

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