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

HRID 637162

반응식

HRID 637162 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 18464541Methyl5-isothiocyanato-2-methoxybenzoate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-4ac3dee6d5d94c8aa6b1ae1554ac0251
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06194406B1

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