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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 69018590, 화합물 → HCID 57976116, 화합물

HRID 1865192
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HRID 1865192 반응식
[CH2:1]([O:3][C:4](=[O:33])[CH:5]([C:13]1[C:18]([N+:19]([O-])=O)=[CH:17][CH:16]=[C:15]([O:22][CH:23]2[CH2:28][CH2:27][N:26]([CH2:29][CH2:30][O:31][CH3:32])[CH2:25][CH2:24]2)[N:14]=1)C(OC(C)(C)C)=O)[CH3:2]>C(O)(C(F)(F)F)=O>[CH2:1]([O:3][C:4](=[O:33])[CH2:5][C:13]1[C:18]([NH2:19])=[CH:17][CH:16]=[C:15]([O:22][CH:23]2[CH2:24][CH2:25][N:26]([CH2:29][CH2:30][O:31][CH3:32])[CH2:27][CH2:28]2)[N:14]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 69018590HCID 69018590, 화합물

생성물 1

HCID 57976116HCID 57976116, 화합물수율 87.6%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

A mixture of 3 (0.856 mmol) in TFA (15 mL) was agitated at room temperature for 20 min. LCMS indicated a mixture of ˜1:1 of the tButyl cleavage/decarboxylation to tButyl and Ethyl cleavage/decarboxylation. The TFA was removed in vacuo. The resulting oil was put up in ethyl acetate and washed with sodium bicarbonate (aq., satd.), brine then dried over MgSO4 and concentrated in vacuo. The free based material (4) was dissolved in ethanol (20 mL) and hydrogenated in the presence of 10% Pd/C (30 mg) at 20 psi on the Parr shaker for 1 hour. The suspension was filtered over celite and concentrated in vacuo yielding an orange-yellow oil (253 mg, 87.4%).

후처리

  • additiona mixture of ˜1:1 of the tButyl cleavage/decarboxylation
  • customThe TFA was removed in vacuo
  • washwashed with sodium bicarbonate (aq., satd.), brine
  • dry with materialthen dried over MgSO4
  • concentrationconcentrated in vacuo
  • dissolutionwas dissolved in ethanol (20 mL) and hydrogenated in the presence of 10% Pd/C (30 mg) at 20 psi on the Parr shaker for 1 hour
  • filtrationThe suspension was filtered over celite and
  • concentrationconcentrated in vacuo
  • 출처 및 근거

    ORD 기록
    ord-48b306552a2847d99461306ab7c33890
    출처 데이터셋
    uspto-grants-2009_12
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07626031B2

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