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Sulfamic Acid → 2-Methoxy-6-(3-methoxyphenyl)-1-naphthoic acid

HRID 1035593
ノート
印刷プレビュー

反応式

HRID 1035593 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:10]2[C:5](=[CH:6][CH:7]=[C:8]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([O:19][CH3:20])[CH:14]=3)[CH:9]=2)[C:4]=1[CH:21]=[O:22].NS(O)(=O)=[O:25].Cl[O-].[Na+]>O.CC(C)=O>[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:10]2[C:5](=[CH:6][CH:7]=[C:8]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([O:19][CH3:20])[CH:14]=3)[CH:9]=2)[C:4]=1[C:21]([OH:25])=[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

6

反応物 3

HCID 5987Sulfamic AcidHCID 23665760Sodium HypochloriteHCID 59443478HCID 59443478、化合物

生成物 1

HCID 594434812-Methoxy-6-(3-methoxyphenyl)-1-naphthoic acid

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒

実験手順

200 mg of the compound 2-methoxy-6-(3-methoxyphenyl)-1-naphthaldehyde (0.68 mmol, 1 eq) is dissolved in a mixture of 8 ml of water and 17 ml of acetone. To the cooled reaction mixture, amidosulfonic acid (H2NSO3H) (1.51 mmol, 2.21 eq) and sodium hypochlorite (0.78 mmol, 1.14 eq) are added. After stirring for 30 min, the acetone is removed in vacuum on a rotary evaporator, and dichloromethane is added. The organic and aqueous phases are separated, and the organic phase is washed three times with saturated sodium chloride solution. After drying and concentrating the organic phase on a rotary evaporator, the desired product was obtained as a yellow solid in quantitative yield (209 mg).

後処理

  1. additionare added
  2. customthe acetone is removed in vacuum on a rotary evaporator, and dichloromethane
  3. additionis added
  4. customThe organic and aqueous phases are separated
  5. washthe organic phase is washed three times with saturated sodium chloride solution
  6. customAfter drying
  7. concentrationconcentrating the organic phase
  8. customon a rotary evaporator

出典と根拠

ORDレコード
ord-2bfff05418004227ae9e8e6e5b0b2ff1
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08546392B2

反応ノート

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