Sodium Carbonate → HCID 15839397、化合物

HRID 2292637ノート

反応式

HRID 2292637 の反応式
[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

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 10375850HCID 10375850、化合物HCID 15839404HCID 15839404、化合物

生成物 1

HCID 15839397HCID 15839397、化合物収率 70.3%

試薬・触媒・溶媒 1

HCID 7909Methyl Isobutyl Ketone溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-53563c9728b3439ab2e85b388f2b6b1f
出典データセット
uspto-grants-1997_11
特許番号
US05684020

反応ノート

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