Allyltributylstannane → HCID 67513193, 화합물

HRID 1519637노트

반응식

HRID 1519637 반응식
Br[C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[C:4]([O:10][CH:11]([F:13])[F:12])[CH:3]=1.[Li+].[Cl-].[CH2:16]([Sn](CCCC)(CCCC)CCCC)[CH:17]=[CH2:18]>C1(C)C=CC=CC=1.CCOC(C)=O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:18]([C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[C:4]([O:10][CH:11]([F:13])[F:12])[CH:3]=1)[CH:17]=[CH2:16]

참가 물질

7

반응물 3

HCID 90628AllyltributylstannaneHCID 433294Lithium ChlorideHCID 711049301261494-95-4

생성물 1

HCID 67513193HCID 67513193, 화합물

시약·촉매·용매 3

HCID 178418397HCID 178418397, 화합물촉매HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 4-bromo-2-(difluoromethoxy)benzonitrile (620 mg, 2.5 mmol) in 30 ml of toluene was added LiCl (322 mg, 7.5 mmol), Pd(PPh3)4 (60 mg), Allyl tributyltin (990 mg, 3.0 mmol), and then the mixture was heated to reflux overnight. After the reaction was completed, the reaction solution was diluted with EtOAc and filtered. The filtrate was concentrated and purified with silica gel column chromatograph to give crude 4-allyl-2-(difluoromethoxy)benzonitrile.

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux overnight
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated
  5. custompurified with silica gel column chromatograph

출처 및 근거

ORD 기록
ord-3e229b525721468dba1e46b024554c34
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073882B2

반응 노트

불러오는 중…