7-(2,6-Dichloro-4-nitrophenoxy)-2,2-dimethyl-2,3-dihydro-1-benzofuran → HCID 13246037, 화합물

HRID 978479노트

반응식

HRID 978479 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N+:21]([O-])=O)[CH:5]=[C:6]([Cl:20])[C:7]=1[O:8][C:9]1[C:17]2[O:16][C:15]([CH3:19])([CH3:18])[CH2:14][C:13]=2[CH:12]=[CH:11][CH:10]=1.[H][H]>C1(C)C=CC=CC=1.[Pt]>[Cl:20][C:6]1[CH:5]=[C:4]([CH:3]=[C:2]([Cl:1])[C:7]=1[O:8][C:9]1[C:17]2[O:16][C:15]([CH3:18])([CH3:19])[CH2:14][C:13]=2[CH:12]=[CH:11][CH:10]=1)[NH2:21]

참가 물질

5

반응물 2

HCID 132459927-(2,6-Dichloro-4-nitrophenoxy)-2,2-dimethyl-2,3-dihydro-1-benzofuranHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 13246037HCID 13246037, 화합물수율 89.6%

시약·촉매·용매 2

HCID 23939Platinum촉매HCID 1140Toluene용매

실험 절차

To a solution of 29.2 g of 3,5-dichloro-4-(2,3-dihydro-2,2-dimethyl-7-benzofuranyloxy)-1-nitrobenzene in 500 ml of toluene was added 2.3 g of 5% platinum on carbon catalyst. This mixture was then charged into a 1 L rocking Parr reactor. The reactor was purged twice with nitrogen then twice with hydrogen, then finally filled with hydrogen to a pressure of 100 psig. The hydrogen pressure was maintained between 75 and 100 psig during the course of the reaction. After hydrogen uptake ceased, the reaction mixture was removed from the reactor. This was filtered through celite. Removal of the solvents afforded 23.95 g of off-white crystals. mp 140°-145° C. NMR (CDCl3): 1.53 (s, 6H), 3.03 (s, 2H), 3.70 (broad s, 2H), 6.2-7.0 (M, 5H, contains singlet at 6.62).

후처리

  1. additionThis mixture was then charged into a 1 L
  2. customThe reactor was purged twice with nitrogen
  3. additiontwice with hydrogen, then finally filled with hydrogen to a pressure of 100 psig
  4. temperatureThe hydrogen pressure was maintained between 75 and 100 psig
  5. customduring the course of the reaction
  6. customthe reaction mixture was removed from the reactor
  7. filtrationThis was filtered through celite
  8. customRemoval of the solvents

출처 및 근거

ORD 기록
ord-1132b06db1084be1827617c6f9096f9a
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04665097

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