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Methyl 3-amino-4-propylbenzoate → HCID 178438014、化合物

HRID 1699900
ノート
印刷プレビュー

反応式

HRID 1699900 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][C:11]=1[CH2:12][CH2:13][CH3:14])[C:5]([O:7][CH3:8])=[O:6].[N:15]([O-])=O.[Na+]>C(O)(=O)C.O>[CH2:13]([C:12]1[C:11]2[C:2](=[CH:3][C:4]([C:5]([O:7][CH3:8])=[O:6])=[CH:9][CH:10]=2)[NH:1][N:15]=1)[CH3:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 22387873Methyl 3-amino-4-propylbenzoateHCID 23668193Sodium Nitrite

生成物 1

HCID 178438014HCID 178438014、化合物収率 45.5%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

To a solution of methyl 3-amino-4-propylbenzoate (5.07 g) in acetic acid (150 ml) was dropwise added a solution of sodium nitrite (2.07 g) in water (5 ml) for 5 min. After stirring for 20 min, the reaction mixture was concentrated, and then toluene and a saturated aqueous sodium hydrogencarbonate solution were added to the residue. The separated toluene layer was dried over sodium sulfate and concentrated. The residue was allowed to stand and partially solidified. The solid was washed with hexane and dried to give the object compound (2.44 g) as a brown solid.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. concentrationthe reaction mixture was concentrated
  2. additiontoluene and a saturated aqueous sodium hydrogencarbonate solution were added to the residue
  3. dry with materialThe separated toluene layer was dried over sodium sulfate
  4. concentrationconcentrated
  5. washThe solid was washed with hexane
  6. customdried

出典と根拠

ORDレコード
ord-943b932b36f3488296b1eb696e414c58
出典データセット
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06348474B1

反応ノート

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