Sodium Carbonate → HCID 15839397, 화합물

HRID 2292637노트

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HRID 2292637 반응식
[CH3:1][O:2][C:3]1[C:4]([N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)=[CH:5][C:6]2[O:10][CH2:9][CH2:8][C:7]=2[CH:11]=1.[CH:18]1([CH2:26][CH2:27]Br)[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=2[CH2:19]1.C(=O)([O-])[O-].[Na+].[Na+]>C(C(C)=O)C(C)C>[CH:18]1([CH2:26][CH2:27][N:15]2[CH2:14][CH2:13][N:12]([C:4]3[C:3]([O:2][CH3:1])=[CH:11][C:7]4[CH2:8][CH2:9][O:10][C:6]=4[CH:5]=3)[CH2:17][CH2:16]2)[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=2[CH2:19]1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 10375850HCID 10375850, 화합물HCID 15839404HCID 15839404, 화합물

생성물 1

HCID 15839397HCID 15839397, 화합물수율 70.3%

시약·촉매·용매 1

HCID 7909Methyl Isobutyl Ketone용매

실험 절차

2.21 g (8.2 mmol) of 4-(2,3-dihydro-5-methoxybenzofuran-6-yl)piperazine (Preparation 1), 1.72 g (8.2 mmol) of 2-(benzocyclobutan-1-yl)-1-bromoethane and 3.48 g (32.8 mmol) of sodium carbonate in 33 ml of methyl isobutyl ketone are heated at reflux for 14 h. The whole is evaporated to dryness, taken up in 200 ml of ethyl acetate and 100 ml of N sodium hydroxide solution and decanted, and the organic phase is washed with 100 ml of a saturated sodium chloride solution. After drying over MgSO4 and evaporation, the residue obtained is chromatographed on silica (eluant: CH2Cl2 /CH3OH: 98/2) to yield 2.1 g of the expected product. By the addition of a 2% fumaric acid solution in ethanol, 1.7 g of the fumarate of the title compound is obtained. M.p. 193°-194° C.

후처리

  1. temperatureat reflux for 14 h
  2. customThe whole is evaporated to dryness
  3. custom100 ml of N sodium hydroxide solution and decanted
  4. washthe organic phase is washed with 100 ml of a saturated sodium chloride solution
  5. dry with materialAfter drying over MgSO4 and evaporation
  6. customthe residue obtained
  7. customis chromatographed on silica (eluant: CH2Cl2 /CH3OH: 98/2)

출처 및 근거

ORD 기록
ord-53563c9728b3439ab2e85b388f2b6b1f
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05684020

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