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Benzyloxyamine hydrochloride → HCID 19026180, 화합물

HRID 1821094
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HRID 1821094 반응식
[CH2:1]([O:8][C:9]1[CH:18]=[CH:17][C:16]2[C:15](=O)[CH2:14][CH2:13][CH2:12][C:11]=2[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[CH2:21]([O:28][NH2:29])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>N1C=CC=CC=1>[CH2:21]([O:28][NH:29][CH:15]1[CH2:14][CH2:13][CH2:12][C:11]2[N:10]=[C:9]([O:8][CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[CH:18]=[CH:17][C:16]1=2)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 102312Benzyloxyamine hydrochlorideHCID 104449772-benzyloxy-7,8-dihydro-6H-quinolin-5-one

생성물 1

HCID 19026180HCID 19026180, 화합물수율 96%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

To the mixture of 2-benzyloxy-7,8-dihydro-6H-quinolin-5-one (37.8 g, 149 mmoL) in pyridine (300 mL) was added O-benzylhydroxylamine hydrochloride (26.2 g, 164 mmoL) and the resulting mixture was stirred at room temperature for 24 h. The reaction was concentrated, diluted with methylene chloride and washed with saturated sodium bicarbonate (×2) and brine (×2). The methylene chloride layer was dried, filtered and concentrated. Purification by column chromatography on silica gel with 5% ethyl acetate in hexane provided the desired product (51.0 g, 96%) as an offwhite solid.

후처리

  1. concentrationThe reaction was concentrated
  2. additiondiluted with methylene chloride
  3. washwashed with saturated sodium bicarbonate (×2) and brine (×2)
  4. dry with materialThe methylene chloride layer was dried
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customPurification by column chromatography on silica gel with 5% ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-e75e3b70f17a45d6bf760a91ebef6a63
출처 데이터셋
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07605265B2

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