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Trifluoroacetic acid → HCID 44129294, 화합물

HRID 1514291
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HRID 1514291 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:12]2[O:16][N:15]=[C:14]([C:17]3[CH:34]=[CH:33][C:20]4[CH2:21][CH2:22][N:23](C(OC(C)(C)C)=O)[CH2:24][CH2:25][C:19]=4[CH:18]=3)[N:13]=2)[CH:5]=[N:6][C:7]=1[O:8][CH:9]([CH3:11])[CH3:10].FC(F)(F)C(O)=O>ClCCl>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([C:12]2[O:16][N:15]=[C:14]([C:17]3[CH:34]=[CH:33][C:20]4[CH2:21][CH2:22][NH:23][CH2:24][CH2:25][C:19]=4[CH:18]=3)[N:13]=2)[CH:5]=[N:6][C:7]=1[O:8][CH:9]([CH3:10])[CH3:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 59403440HCID 59403440, 화합물

생성물 1

HCID 44129294HCID 44129294, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1,1-Dimethylethyl 7-(5-{5-chloro-6-[(1-methylethyl)oxy]-3-pyridinyl}-1,2,4-oxadiazol-3-yl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (Preparation 96) (305 mg, 0.629 mmol) in dichloromethane (2 mL) at room temperature was treated with trifluoroacetic acid (1 ml, 12.98 mmol) and the mixture stirred for 1 hr. The reaction mixture was concentrated and the residue partitioned between 2M NaOH and ethyl acetate. The ethyl acetate extract was washed with brine, dried and concentrated to a colourless gum which slowly crystallized, to give the title compound free base (229 mgs).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. customthe residue partitioned between 2M NaOH and ethyl acetate
  3. extractionThe ethyl acetate extract
  4. washwas washed with brine
  5. customdried
  6. concentrationconcentrated to a colourless gum which
  7. customslowly crystallized

출처 및 근거

ORD 기록
ord-5bf1ae772bb14e71b25df0922b755d84
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08222245B2

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