Potassium Sodium Tartrate → HCID 68989883, 화합물

HRID 69483

반응식

HRID 69483 반응식
C[Al](C)C.[O:5]1[C:9]2([CH2:13][CH2:12][N:11]([C:14]3[CH:19]=[CH:18][C:17]([NH2:20])=[CH:16][C:15]=3[F:21])[CH2:10]2)[O:8][CH2:7][CH2:6]1.[CH3:22][O:23][C:24]1[CH:25]=[C:26]2[C:31](=[CH:32][CH:33]=1)[C:30](=[O:34])[O:29][CH2:28][CH2:27]2.[C@H](O)(C([O-])=O)[C@@H](O)C([O-])=O.[Na+].[K+]>C1(C)C=CC=CC=1.C(Cl)Cl>[O:8]1[C:9]2([CH2:13][CH2:12][N:11]([C:14]3[CH:19]=[CH:18][C:17]([NH:20][C:30](=[O:34])[C:31]4[CH:32]=[CH:33][C:24]([O:23][CH3:22])=[CH:25][C:26]=4[CH2:27][CH2:28][OH:29])=[CH:16][C:15]=3[F:21])[CH2:10]2)[O:5][CH2:6][CH2:7]1

참가 물질

7

반응물 4

HCID 9357Potassium Sodium TartrateHCID 124011826-Methoxy-3,4-dihydro-1H-2-benzopyran-1-oneHCID 16682925TrimethylaluminumHCID 211054314-(1,4-Dioxa-7-azaspiro[4.4]non-7-yl)-3-fluorophenylamine

생성물 1

HCID 68989883HCID 68989883, 화합물

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

A 2M solution of trimethylaluminum in toluene (14.9 mL) was added dropwise at 0° C. to a solution of 4-(1,4-dioxa-7-aza-spiro[4.4]non-7-yl)-3-fluorophenylamine (5.3 g) in methylene chloride (100.8 mL). The reaction mixture was stirred for 15 min at 0° C. and then for 30 min at room temperature. Then a solution of 6-methoxy-isochroman-1-one (3.8 g) in methylene chloride (40 mL) was added dropwise. The reaction mixture was stirred overnight at room temperature. Then saturated Rochelle salt solution was carefully added and the mixture was stirred for 1 h at room temperature. The aqueous phase was extracted several times with methylene chloride. 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 416.17 (C22H25FN2O5); MS (ESI): 417 (M+H+).

후처리

  1. waitfor 30 min at room temperature
  2. stirringThe reaction mixture was stirred overnight at room temperature
  3. stirringthe mixture was stirred for 1 h at room temperature
  4. extractionThe aqueous phase was extracted several times with methylene chloride
  5. dry with materialdried over sodium sulfate
  6. customthe solvent was removed in vacuum
  7. customIn this way the product was obtained with molecular weight 416.17 (C22H25FN2O5)

출처 및 근거

ORD 기록
ord-a97c7772dc6149feb9d3501c939816d1
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822495B2

연결된 노트

불러오는 중…