Thionyl Chloride → 5-Bromo-2,4-dimethoxybenzoyl chloride

HRID 1967447노트

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HRID 1967447 반응식
[Br:1][C:2]1[C:3]([O:13][CH3:14])=[CH:4][C:5]([O:11][CH3:12])=[C:6]([CH:10]=1)[C:7](O)=[O:8].S(Cl)([Cl:17])=O>C1(C)C=CC=CC=1>[Br:1][C:2]1[C:3]([O:13][CH3:14])=[CH:4][C:5]([O:11][CH3:12])=[C:6]([CH:10]=1)[C:7]([Cl:17])=[O:8]

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 135050975-Bromo-2,4-dimethoxybenzoic acid

생성물 1

HCID 135050985-Bromo-2,4-dimethoxybenzoyl chloride

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
75 °C

실험 절차

Under a nitrogen atmosphere, 5-bromo-2,4-dimethoxybenzoic acid (40.0 g) was suspended in toluene solution (DMF concentration: 300 ppm, 200 mL). To the suspension was added dropwise thionyl chloride (21.9 g) at 75° C. After stirring at 75° C. for 1 hr, completion of the reaction was confirmed by HPLC. Toluene and excess thionyl chloride were evaporated under reduced pressure. Toluene (100 mL) was added to the concentrated residue, and the mixture was concentrated again under reduced pressure. THF (100 mL) was added to the obtained 5-bromo-2,4-dimethoxybenzoic acid chloride, which was directly used in the next step.

후처리

  1. customToluene and excess thionyl chloride were evaporated under reduced pressure
  2. additionToluene (100 mL) was added to the concentrated residue
  3. concentrationthe mixture was concentrated again under reduced pressure
  4. additionTHF (100 mL) was added to the obtained 5-bromo-2,4-dimethoxybenzoic acid chloride, which

출처 및 근거

ORD 기록
ord-e0e3d20ee74a4a729e4c0e64db93c569
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08420821B2

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