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Hydroxylamine → HCID 11222341、化合物

HRID 2076423
ノート
印刷プレビュー

反応式

HRID 2076423 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 787HydroxylamineHCID 13655816HCID 13655816、化合物

生成物 1

HCID 11222341HCID 11222341、化合物収率 35%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e002d19708174c05b7d5624708617ab4
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07923579B2

反応ノート

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