3-Bromo-4-(trifluoromethoxy)benzoic acid → HCID 67211313, 화합물

HRID 2040532노트

반응식

HRID 2040532 반응식
Br[C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][C:12]([F:15])([F:14])[F:13])[C:5]([OH:7])=[O:6].[C:16]([Cu])#[N:17]>CN1CCCC1=O.ClCCl>[C:16]([C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][C:12]([F:15])([F:14])[F:13])[C:5]([OH:7])=[O:6])#[N:17]

참가 물질

5

반응물 2

HCID 202740913-Bromo-4-(trifluoromethoxy)benzoic acidHCID 178418546HCID 178418546, 화합물

생성물 1

HCID 67211313HCID 67211313, 화합물수율 86.3%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
200 °C

실험 절차

3-Bromo-4-(trifluoromethoxy)benzoic acid (1.4 g, 4.91 mmol) and cyanocopper (0.572 g, 6.39 mmol) were mixed in N-methyl-2-pyrrolidinone (NMP) (14 mL). The mixture was heated in a microwave at 200° C. for 2 h. The reaction was diluted with dichloromethane (150 mL). Celite® was added and the mixture was stirred vigorously for 10 min. The solids were removed by filtration. The organic layer was washed with water (125 mL) and concentrated. The residue was purified by HPLC to give the title compound as an off-white solid (0.979 g). LCMS m/z=232.3 [M+H]+.

후처리

  1. additionCelite® was added
  2. customThe solids were removed by filtration
  3. washThe organic layer was washed with water (125 mL)
  4. concentrationconcentrated
  5. customThe residue was purified by HPLC

출처 및 근거

ORD 기록
ord-38dcfd3944dd4869a462efdb01082ce5
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08580841B2

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