Methyl 5-amino-o-anisate → Methyl5-isothiocyanato-2-methoxybenzoate

HRID 637162

反応式

HRID 637162 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:10]([NH2:13])=[CH:9][C:4]=1[C:5]([O:7][CH3:8])=[O:6].C1C=C(O[C:21](OC2N=CC=CC=2)=[S:22])N=CC=1>ClCCl>[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:10]([N:13]=[C:21]=[S:22])=[CH:9][C:4]=1[C:5]([O:7][CH3:8])=[O:6]

参加物

4

反応物 2

HCID 89843Methyl 5-amino-o-anisateHCID 719784O,O-Dipyridin-2-yl carbonothioate

生成物 1

HCID 18464541Methyl5-isothiocyanato-2-methoxybenzoate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

According to the method of Tet. Let., 26, 1661 (1985), combine methyl 2-methoxy-5-aminobenzoate (0.5 g, 2.76 mmol) and di-2-pyridyl thionocarbonate (0.64 g, 2.76 mmol) in dichloromethane (10 mL). After 30 minutes, dilute the reaction mixture with dichloromethane and extract five times with water. Dry the organic layer over Na2SO4, filter, and concentrate in vacuo to give methyl 2-methoxy-5-isothiocyanatobenzoate: Rf=0.51 (silica gel, dichloromethane).

後処理

  1. extractionextract five times with water
  2. dry with materialDry the organic layer over Na2SO4
  3. filtrationfilter
  4. concentrationconcentrate in vacuo

出典と根拠

ORDレコード
ord-4ac3dee6d5d94c8aa6b1ae1554ac0251
出典データセット
uspto-grants-2001_02
特許番号
US06194406B1

関連ノート

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