Water → HCID 178480023, 화합물

HRID 38492노트

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HRID 38492 반응식
C1C=CC2N(O)N=NC=2C=1.Cl.[CH3:12][N:13]1[CH:17]=[C:16]([C:18]2[CH:19]=[C:20]3[C:30](=[CH:31][CH:32]=2)[O:29][C:23]2([CH2:28][CH2:27][NH:26][CH2:25][CH2:24]2)[CH2:22][C:21]3=[O:33])[CH:15]=[N:14]1.[CH:34]1([C:37]2[CH:38]=[CH:39][CH:40]=[C:41]3[C:46]=2[N:45]=[C:44]([C:47](O)=[O:48])[CH:43]=[C:42]3[OH:50])[CH2:36][CH2:35]1.O>CN(C=O)C>[CH:34]1([C:37]2[CH:38]=[CH:39][CH:40]=[C:41]3[C:46]=2[N:45]=[C:44]([C:47]([N:26]2[CH2:25][CH2:24][C:23]4([CH2:22][C:21](=[O:33])[C:20]5[C:30](=[CH:31][CH:32]=[C:18]([C:16]6[CH:15]=[N:14][N:13]([CH3:12])[CH:17]=6)[CH:19]=5)[O:29]4)[CH2:28][CH2:27]2)=[O:48])[CH:43]=[C:42]3[OH:50])[CH2:35][CH2:36]1

참가 물질

6

반응물 4

HCID 962WaterHCID 757711-HydroxybenzotriazoleHCID 667825466-(1-Methyl-1H-pyrazol-4-yl)spiro[chroman-2,4'-piperidin]-4-one hydrochlorideHCID 178524587HCID 178524587, 화합물

생성물 1

HCID 178480023HCID 178480023, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

TEA (0.657 ml, 4.71 mmol) was added to a stirred mixture of HOBT (313 mg, 2.04 mmol), WSCDI (361 mg, 1.89 mmol), 6-(1-methyl-1H-pyrazol-4-yl)spiro[chroman-2,4′-piperidin]-4-one hydrochloride (629 mg, 1.89 mmol) and 8-cyclopropyl-4-hydroxyquinoline-2-carboxylic acid (360 mg, 1.57 mmol) in DMF (3.5 ml) and the mixture was stirred at room temperature overnight. The reaction mixture was poured into water (20 ml) and stirred for 30 min. The resulted precipitate was filtered, washed with water and the solid was dried in vacuo at 70° C. The crude product was purified by silicagel column chromatography (CHCl3/AcOEt) to give intended compound as a pale brown solid.

후처리

  1. stirringstirred for 30 min
  2. filtrationThe resulted precipitate was filtered
  3. washwashed with water
  4. customthe solid was dried in vacuo at 70° C
  5. customThe crude product was purified by silicagel column chromatography (CHCl3/AcOEt)
  6. customto give

출처 및 근거

ORD 기록
ord-ae09d597526b4d1695d38fdc5e65746c
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524730B2

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