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Phthalimide → HCID 21076931, 화합물

HRID 1455161
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HRID 1455161 반응식
[C:1]1(=[O:11])[NH:5][C:4](=O)[C:3]2=[CH:7][CH:8]=[CH:9][CH:10]=[C:2]12.C(N1C(=O)[C:23]([CH3:26])=[C:22]([CH3:27])[N:21]=[C:20]1[C@H:28]([N:32]([CH2:42][CH2:43][N:44]1C(=O)C2C(=CC=CC=2)C1=O)[C:33](=O)[C:34]1[CH:39]=[CH:38][C:37]([CH3:40])=[CH:36][CH:35]=1)[CH:29]([CH3:31])[CH3:30])C1C=CC=CC=1.O.NN>C(O)C>[CH2:4]([N:5]1[C:1](=[O:11])[C:23]([CH3:26])=[C:22]([CH3:27])[N:21]=[C:20]1[C@H:28]([N:32]1[CH2:42][CH2:43][N:44]=[C:33]1[C:34]1[CH:35]=[CH:36][C:37]([CH3:40])=[CH:38][CH:39]=1)[CH:29]([CH3:31])[CH3:30])[C:3]1[CH:2]=[CH:10][CH:9]=[CH:8][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6809PhthalimideHCID 24654Hydrazine hydrate (1:1)HCID 69016795HCID 69016795, 화합물

생성물 1

HCID 21076931HCID 21076931, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
120 °C

실험 절차

The phthalimide protected amine, N—[(R)-1-(1-benzyl-4,5-dimethyl-6-oxo-1,6-dihydro-pyrimidin-2-yl)-2-methyl-propyl]-N-[2-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-ethyl]-4-methyl-benzamide, (0.075 g, 0.13 mMol) was treated with hydrazine monohydrate (0.013 mL, 0.26 mMol) in ethanol (1 mL) at 70° C. for 12 h. The reaction was filtered, concentrated under vacuum and dissolved in toluene (1 mL) and heated to 120° C. for 20 h. The reaction was concentrated under vacuum, taken up in CH3CN and purified by reverse phase HPLC (YMC, ODS-A, 20 min, 5-90% gradient, CH3CN:H2O, 0.1% TFA) The fractions were collected and evaporated to give the title compound as a clear oil. (0.016 g): MS (ES) m/e 429.4 (M+H)+.

후처리

  1. filtrationThe reaction was filtered
  2. concentrationconcentrated under vacuum
  3. dissolutiondissolved in toluene (1 mL)
  4. concentrationThe reaction was concentrated under vacuum
  5. custompurified by reverse phase HPLC (YMC, ODS-A, 20 min, 5-90% gradient, CH3CN:H2O, 0.1% TFA) The fractions
  6. customwere collected
  7. customevaporated

출처 및 근거

ORD 기록
ord-16e3537473fc4b71b1c47b4318959f9b
출처 데이터셋
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07482343B2

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