p-Toluenesulfonic acid → HCID 68988102, 화합물

HRID 69461노트

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HRID 69461 반응식
O1[C:5]2([CH2:9][CH2:8][N:7]([C:10]3[CH:15]=[CH:14][C:13]([N:16]4[CH2:25][CH2:24][C:23]5[C:18](=[CH:19][CH:20]=[C:21]([O:26][CH2:27][C@@H:28]6[CH2:32][CH2:31][CH2:30][O:29]6)[CH:22]=5)[C:17]4=[O:33])=[CH:12][C:11]=3[F:34])[CH2:6]2)[O:4]CC1.C1(C)C=CC(S(O)(=O)=O)=CC=1>CC(C)=O.O>[F:34][C:11]1[CH:12]=[C:13]([N:16]2[CH2:25][CH2:24][C:23]3[C:18](=[CH:19][CH:20]=[C:21]([O:26][CH2:27][C@@H:28]4[CH2:32][CH2:31][CH2:30][O:29]4)[CH:22]=3)[C:17]2=[O:33])[CH:14]=[CH:15][C:10]=1[N:7]1[CH2:8][CH2:9][C:5](=[O:4])[CH2:6]1

참가 물질

4

반응물 2

HCID 6101p-Toluenesulfonic acidHCID 68992282HCID 68992282, 화합물

생성물 1

HCID 68988102HCID 68988102, 화합물

시약·촉매·용매 1

HCID 18366337Propan-2-one--water (1/1)용매

반응 조건

온도
70 °C

실험 절차

A mixture of 2-[4-(1,4-dioxa-7-aza-spiro[4.4]non-7-yl)-3-fluorophenyl]-6-[(S)-1-(tetrahydrofuran-2-yl)methoxy]-3,4-dihydro-2H-isoquinolin-1-one (8.4 g) and p-toluenesulfonic acid (3.4 g) in acetone/water (80 mL/40 mL) was heated for 12 h at 70° C. Then the acetone was removed in vacuum and the aqueous phase was neutralized with sodium hydrogencarbonate solution and then extracted several times with ethyl acetate. The organic phases were combined, dried over sodium sulfate and the solvent was removed in vacuum. In this way the product was obtained with molecular weight 424.47 (C24H25FN2O4); MS (ESI): 425 (M+H+).

후처리

  1. customThen the acetone was removed in vacuum
  2. extractionextracted several times with ethyl acetate
  3. dry with materialdried over sodium sulfate
  4. customthe solvent was removed in vacuum
  5. customIn this way the product was obtained with molecular weight 424.47 (C24H25FN2O4)

출처 및 근거

ORD 기록
ord-ad83ca4a916b450ea9ee7c3e86fcb9db
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822495B2

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