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Phosphorus oxide (P4O10) → HCID 86600129, 화합물

HRID 271524
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HRID 271524 반응식
C(OC([N:11]1[CH2:16][CH2:15][CH:14]([C:17](=[O:40])[CH2:18][CH:19]([C:28]2[CH:29]=[C:30]3[C:34](=[CH:35][CH:36]=2)[C:33](=[N:37][O:38][CH3:39])[CH2:32][CH2:31]3)[C:20](=O)[C:21]2[CH:26]=[CH:25][N:24]=[CH:23][CH:22]=2)[CH2:13][CH2:12]1)=O)C1C=CC=CC=1.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>CS(O)(=O)=O>[CH3:39][O:38][N:37]=[C:33]1[C:34]2[C:30](=[CH:29][C:28]([C:19]3[CH:18]=[C:17]([CH:14]4[CH2:15][CH2:16][NH:11][CH2:12][CH2:13]4)[O:40][C:20]=3[C:21]3[CH:26]=[CH:25][N:24]=[CH:23][CH:22]=3)=[CH:36][CH:35]=2)[CH2:31][CH2:32]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14812Phosphorus oxide (P4O10)HCID 866001284-[3-(1-Methoxyimino-indan-5-yl)-4-oxo-4-pyridin-4-yl-butanoyl]-piperidine-1-carboxylic acid benzyl ester

생성물 1

HCID 86600129HCID 86600129, 화합물수율 32%

시약·촉매·용매 1

HCID 6395Methanesulfonic Acid용매

실험 절차

The product of Step 3 (3.0 g, 5.5 mmol) was added to a stirred suspension of phosphorus pentoxide (8 g) in dry methane sulphonic acid (50 ml). After stirring at room temperature for 4 hours the reaction mixture was cautiously poured into a stirred solution of ice cold 50% aqueous sodium hydroxide (final pH 10). The mixture was extracted with chloroform, washed with water and brine, dried and concentrated in vacuo and the residue purified by silica gel chromatography to give the title compound (0.66 g, 32%); MS(ES+) m/e 388 [M+H]+.

후처리

  1. extractionThe mixture was extracted with chloroform
  2. washwashed with water and brine
  3. customdried
  4. concentrationconcentrated in vacuo
  5. customthe residue purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-0d345896a9194f259acc2f9731cdc511
출처 데이터셋
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07452906B2

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