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Hydroxylamine → HCID 21293763, 화합물

HRID 620815
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HRID 620815 반응식
C([O:4][N:5]([CH:9]([C:11]1[CH:12]=[CH:13][C:14]2[C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=3[O:16][C:15]=2[CH:23]=1)[CH3:10])[C:6](=[O:8])[CH3:7])(=O)C.C(OC(=O)C)(=O)C.NO.C(N(CC)CC)C>C(Cl)Cl>[OH:4][N:5]([CH:9]([C:11]1[CH:12]=[CH:13][C:14]2[C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=3[O:16][C:15]=2[CH:23]=1)[CH3:10])[C:6](=[O:8])[CH3:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 787HydroxylamineHCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 21293762HCID 21293762, 화합물

생성물 1

HCID 21293763HCID 21293763, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

N-acetoxy-N-(1-dibenzofur-3-ylethyl) acetamide. Acetic anhydride (9.0 mL) was added to a solution of the crude hydroxylamine, prepared as in step c, and triethyl amine (12.4 mL) in methylene chloride (50 mL). The reaction was stirred overnight, then washed with cold water and 3 N HCl. The methylene chloride layer was dried (Na2SO4) and concentrated to give a yellowish oil. This residue was chromatographed on 100 g of silica gel, eluting with 20% ethyl acetate in hexanes to give the desired product.

후처리

  1. washwashed with cold water and 3 N HCl
  2. dry with materialThe methylene chloride layer was dried (Na2SO4)
  3. concentrationconcentrated
  4. customto give a yellowish oil
  5. customThis residue was chromatographed on 100 g of silica gel
  6. washeluting with 20% ethyl acetate in hexanes

출처 및 근거

ORD 기록
ord-adea5f33ead14d32a4f1d376c0b19330
출처 데이터셋
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04822811

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