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Hydrochloric Acid → HCID 19786539, 화합물

HRID 1646715
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HRID 1646715 반응식
CN([CH2:4][N:5]([CH3:7])[CH3:6])C.FC(F)(F)C(O)=O.[C:15]1([C:21]2[C:25]3[C:26](=[O:30])[CH2:27][CH2:28][CH2:29][C:24]=3[O:23][N:22]=2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[ClH:31]>>[ClH:31].[CH3:7][N:5]([CH2:4][CH:27]1[C:26](=[O:30])[C:25]2[C:21]([C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=3)=[N:22][O:23][C:24]=2[CH2:29][CH2:28]1)[CH3:6]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 313Hydrochloric Acid2회HCID 5829N,N,N',N'-TetramethylmethanediamineHCID 6422Trifluoroacetic acidHCID 12344070HCID 12344070, 화합물

생성물 1

HCID 19786539HCID 19786539, 화합물

반응 조건

온도
-10 °C

실험 절차

Bis-dimethylaminomethane (0.51 g) was added to 2.5 ml of trifluoroacetic acid which had been previously chilled to -10° C. 6,7-Dihydro-3-phenyl-1,2-benzisoxazol-4(5H)-one (1.0 g) was then added and the reaction was warmed for 1 hour at 100° C. and then allowed to stand an additional 2 days at room temperature. The reaction mixture was poured into 5% HCl and washed with ether, after which the aqueous phase was treated with solid sodium bicarbonate until basic. Extraction with ether followed by drying and concentration gave an oil. The hydrochloride was formed in ethereal HCl and was recrystallized from dichloromethane/ether to give 0.95 g of 6,7-dihydro-5-dimethylaminomethyl-3-phenyl-1,2-benzisoxazol-4(5H)-one hydrochloride, m.p. 178°-180° C.

후처리

  1. temperaturethe reaction was warmed for 1 hour at 100° C.
  2. washwashed with ether
  3. additionafter which the aqueous phase was treated with solid sodium bicarbonate until basic
  4. extractionExtraction with ether
  5. customby drying
  6. concentrationconcentration
  7. customgave an oil

출처 및 근거

ORD 기록
ord-146d0cbf56d04b52959c98c6542a93d1
출처 데이터셋
uspto-grants-1993_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05180834

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