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Phosphoric Acid → HCID 178456921, 화합물

HRID 1620686
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HRID 1620686 반응식
[F:1][C:2]([F:32])([F:31])[C:3]1[CH:26]=[C:25]([C:27]([F:30])([F:29])[F:28])[CH:24]=[CH:23][C:4]=1[CH2:5][N:6]1[CH2:11][CH2:10][CH:9](/[CH:12]=[C:13]2/[C:14]([NH:19][CH2:20][C:21]#[CH:22])=[N:15][C:16](=[O:18])[S:17]/2)[CH2:8][CH2:7]1.[P:33](=[O:37])([OH:36])([OH:35])[OH:34]>C(O)C>[P:33]([OH:37])([OH:36])([OH:35])=[O:34].[F:32][C:2]([F:1])([F:31])[C:3]1[CH:26]=[C:25]([C:27]([F:29])([F:30])[F:28])[CH:24]=[CH:23][C:4]=1[CH2:5][N:6]1[CH2:7][CH2:8][CH:9](/[CH:12]=[C:13]2/[C:14]([NH:19][CH2:20][C:21]#[CH:22])=[N:15][C:16](=[O:18])[S:17]/2)[CH2:10][CH2:11]1
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참가 물질

4

반응물 2

HCID 1004Phosphoric AcidHCID 178456914HCID 178456914, 화합물

생성물 1

HCID 178456921HCID 178456921, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
60 °C

실험 절차

To a solution of (5Z)-5-({1-[2,4-bis(trifluoromethyl)benzyl]piperidin-4-yl}methylidene)-4-(prop-2-yn-1-ylamino)-1,3-thiazol-2(5H)-one (1 g) in ethanol (15 mL) was added phosphoric acid (0.14 mL). The reaction mixture was stirred at 60° C. for 1 hr, the solvent was evaporated under reduced pressure, and the residue was recrystallized from ethanol/heptane. The crystals were suspended in ethyl acetate at 65° C., and the precipitate was is collected by filtration to give the title compound (0.95 g).

후처리

  1. customthe solvent was evaporated under reduced pressure
  2. customthe residue was recrystallized from ethanol/heptane
  3. customwere suspended in ethyl acetate at 65° C.
  4. filtrationthe precipitate was is collected by filtration

출처 및 근거

ORD 기록
ord-8b9dc2d1231a44c8b5529e1bd4422ea9
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772277B2

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