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Trifluoroacetic acid → HCID 70624241, 화합물

HRID 2420165
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HRID 2420165 반응식
[O:1]=[C:2]([O:28][C:29]1[CH:37]=[CH:36][CH:35]=[C:34]2[C:30]=1[CH2:31][CH2:32][CH2:33]2)[CH:3]1[O:8][CH2:7][CH2:6][N:5](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[CH2:4]1.FC(F)(F)C(O)=O.N1CCOCC1.C(=O)([O-])O.[Na+]>O>[O:1]=[C:2]([O:28][C:29]1[CH:37]=[CH:36][CH:35]=[C:34]2[C:30]=1[CH2:31][CH2:32][CH2:33]2)[CH:3]1[O:8][CH2:7][CH2:6][NH:5][CH2:4]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6422Trifluoroacetic acidHCID 8083MorpholineHCID 516892Sodium BicarbonateHCID 70624682HCID 70624682, 화합물

생성물 1

HCID 70624241HCID 70624241, 화합물수율 89.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 1 g. of 2-(1-oxo-4-indanyloxymethyl)-4-triphenylmethyl morpholine was added 10 ml. of trifluoroacetic acid under ice-cooling to dissolve the morpholine and 10 ml. of water was immediately added to the solution followed by stirring for 15 minutes at 5°-10° C. Then, after neutralizing the reaction mixture with sodium hydrogencarbonate, the product was extracted with chloroform. Then, the extract was washed with water, dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The sticky residue formed was subjected to a silica gel column chromatography (column diameter 3 cm., height 7 cm,) and from the fraction recovered therefrom using a 98 : 2 mixture of chloroform and methanol as an eluting solution, 0.45 g. (yield 89.1%) of sticky 2-(1-oxo-4-indanyloxymethyl)morpholine was obtained.

후처리

  1. extractionthe product was extracted with chloroform
  2. washThen, the extract was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe sticky residue formed
  6. customrecovered
  7. additiona 98 : 2 mixture of chloroform and methanol as an eluting solution, 0.45 g

출처 및 근거

ORD 기록
ord-0866adc41828474e81b679812216228d
출처 데이터셋
uspto-grants-1978_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04109088

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