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Hydroxylamine → HCID 11222341, 화합물

HRID 2076423
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HRID 2076423 반응식
[CH3:1][C:2]1([CH3:27])[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]2[CH:7]=[C:6]([C:14]([NH:16][C:17]3[CH:26]=[CH:25][C:20]([C:21](OC)=[O:22])=[CH:19][CH:18]=3)=[O:15])[CH:5]=[CH:4][C:3]1=2.[NH2:28][OH:29]>CO>[OH:29][NH:28][C:21]([C:20]1[CH:19]=[CH:18][C:17]([NH:16][C:14]([C:6]2[CH:5]=[CH:4][C:3]3[C:2]([CH3:27])([CH3:1])[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]=3[CH:7]=2)=[O:15])=[CH:26][CH:25]=1)=[O:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 787HydroxylamineHCID 13655816HCID 13655816, 화합물

생성물 1

HCID 11222341HCID 11222341, 화합물수율 35%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

To a solution of methyl 4-(5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene-2-carboxamido)benzoate 3 (0.200 g, 0.5 mmol) in MeOH (2 mL) was added an hydroxylamine solution (1.76 M, 2 mL) in MeOH and the reaction mixture was stirred 1 h at RT under magnetic stirring. The reaction mixture was adjusted to pH=5, concentrated and the residue was partitioned between EtOAc and H2O. The organic layer was dried with Na2SO4 and the product was crystallized by dissolving the mixture at 80° C. in CH3CN to give N-(4-(hydroxycarbamoyl)phenyl)-5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene-2-carboxamide EHT 3741 (0.070 g, 35% yield) as a pale red solid.

후처리

  1. concentrationconcentrated
  2. customthe residue was partitioned between EtOAc and H2O
  3. dry with materialThe organic layer was dried with Na2SO4
  4. customthe product was crystallized
  5. dissolutionby dissolving the mixture at 80° C. in CH3CN

출처 및 근거

ORD 기록
ord-e002d19708174c05b7d5624708617ab4
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07923579B2

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