Triethylamine → Methyl 2-diphenylphosphino-1-naphthoate

HRID 430042노트

반응식

HRID 430042 반응식
[C:1]1([PH:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.FC(F)(F)S(O[C:20]1[CH:29]=[CH:28][C:27]2[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=2)[C:21]=1[C:30]([O:32][CH3:33])=[O:31])(=O)=O.C(N(CC)CC)C>CN(C=O)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[C:8]1([P:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:20]2[CH:29]=[CH:28][C:27]3[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=3)[C:21]=2[C:30]([O:32][CH3:33])=[O:31])[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 70017DiphenylphosphineHCID 11034997Methyl 2-trifluoromethanesulfonyloxy-1-naphthoate

생성물 1

HCID 11760420Methyl 2-diphenylphosphino-1-naphthoate

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 6228Dimethylformamide용매

실험 절차

Diphenylphosphine (0.72 mL, 4.14 mmol, 1 eq) was added to a stirred solution of methyl 2-trifluoromethanesulfonyloxy-1-naphthoate (1.384 g, 4.14 mmol, 1 eq), triethylamine (0.64 mL, 4.59 mmol, 1.1 eq) and palladium acetate (0.005 g, 0.02 mmol, 0.005 eq) in degassed DMF (10 mL) instantly giving a red coloration. The solution was heated at reflux under nitrogen for 17 hours. The blood-red solution was allowed to cool and an aliquot taken for NMR analysis.

후처리

  1. custominstantly giving a red coloration
  2. temperatureThe solution was heated
  3. temperatureat reflux under nitrogen for 17 hours
  4. temperatureto cool

출처 및 근거

ORD 기록
ord-cd3c16b55b584541a2e23cf78ca202f1
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06320068B1

반응 노트

불러오는 중…