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Triphenylphosphine → HCID 136347238, 화합물

HRID 601322
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HRID 601322 반응식
[N:1]([CH2:4][C:5]1[C:13]2[S:12](=[O:15])(=[O:14])[N:11]=[C:10]([C:16]3[C:17](=[O:34])[N:18]([CH2:27][C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)[C:19]4[C:24]([C:25]=3[OH:26])=[CH:23][CH:22]=[CH:21][CH:20]=4)[NH:9][C:8]=2[S:7][CH:6]=1)=[N+]=[N-].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>N1C=CC=CC=1.[OH-].[NH4+]>[NH2:1][CH2:4][C:5]1[C:13]2[S:12](=[O:15])(=[O:14])[N:11]=[C:10]([C:16]3[C:17](=[O:34])[N:18]([CH2:27][C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)[C:19]4[C:24]([C:25]=3[OH:26])=[CH:23][CH:22]=[CH:21][CH:20]=4)[NH:9][C:8]=2[S:7][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 11776TriphenylphosphineHCID 136358490HCID 136358490, 화합물

생성물 1

HCID 136347238HCID 136347238, 화합물수율 78%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 14923Ammonium Hydroxide용매

실험 절차

To the solution of the product of Example 344 (136.2 mg, 0.28 mmol) in pyridine (1.68 mL) and concentrated ammonium hydroxide (1.12 mL) was added triphenylphosphine (145 mg, 0.55 mmol) at room temperature. The solution was stirred at room temperature overnight and concentrated in vacuo. The residue was diluted with toluene and the solid was filtered to give the title compound as a light brown solid (100.78 mg, 78%). MS (ESI+) m/z 467 (M+H)+. 1H NMR (300 MHz, DMSO-d6) δ 4.10 (s, 2 H) 5.41 (br s, 2 H) 7.07-7.32 (m, 8 H) 7.43 (m, 1 H) 8.10 (dd, J=7.91, 1.65 Hz, 1 H).

후처리

  1. concentrationconcentrated in vacuo
  2. additionThe residue was diluted with toluene
  3. filtrationthe solid was filtered

출처 및 근거

ORD 기록
ord-ef968bd7c6a04b25a909e880e83ddd10
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07902203B2

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