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Triethylamine → HCID 89419882, 화합물

HRID 920182
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HRID 920182 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-])=O)=[CH:4][C:3]=1[C@@:11]1([CH3:23])[N:19]=[C:18]([NH2:20])[C:14]2([CH2:17][CH2:16][CH2:15]2)[S:13](=[O:22])(=[O:21])[CH2:12]1.C(N(CC)CC)C>C(O)C.[Pd]>[NH2:8][C:5]1[CH:6]=[CH:7][C:2]([F:1])=[C:3]([C@@:11]2([CH3:23])[N:19]=[C:18]([NH2:20])[C:14]3([CH2:17][CH2:16][CH2:15]3)[S:13](=[O:21])(=[O:22])[CH2:12]2)[CH:4]=1
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참가 물질

5

반응물 2

HCID 8471TriethylamineHCID 89419880HCID 89419880, 화합물

생성물 1

HCID 89419882HCID 89419882, 화합물수율 80.5%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

반응 조건

온도
23 °C

실험 절차

To a solution of (R)-7-(2-fluoro-5-nitro-phenyl)-7-methyl-5,5-dioxo-5λ6-thia-8-aza-spiro[3.5]non-8-en-9-ylamine (470 mg, 1.38 mmol, Eq: 1.00) in ethanol (10 ml) was added at 23° C. under inert atmosphere triethylamine (139 mg, 192 μl, 1.38 mmol, Eq: 1.00) and after inertisation Pd/C 10% (62.9 mg, 59.1 μmol, Eq: 0.1). The suspension was set under hydrogen (balloon) and stirred at 23° C. for 1 hour. The catalyst was filtered off, washed three times with ethanol and evaporated to give the crude (R)-7-(5-amino-2-fluoro-phenyl)-7-methyl-5,5-dioxo-5λ6-thia-8-aza-spiro[3.5]non-8-en-9-ylamine (345 mg, 1.11 mmol, 80.5% yield) as a light brown solid. MS (ISP): m/z=312.5 [M+H]+.

후처리

  1. filtrationThe catalyst was filtered off
  2. washwashed three times with ethanol
  3. customevaporated

출처 및 근거

ORD 기록
ord-01f9823823da44cabf5adeac17397b67
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09273042B2

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