Phenylacetyl chloride → HCID 14348999、化合物

HRID 346053ノート

反応式

HRID 346053 の反応式
C(O)(=O)C(O)=O.[F:7][C:8]([F:28])([F:27])[C:9]1[CH:26]=[CH:25][C:12]([O:13][CH:14]2[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=3[CH2:18][CH2:17][NH:16][CH2:15]2)=[CH:11][CH:10]=1.C(N(CC)CC)C.[C:36]1([CH2:42][C:43](Cl)=[O:44])[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1>C(Cl)(Cl)Cl>[C:36]1([CH2:42][C:43]([N:16]2[CH2:15][CH:14]([O:13][C:12]3[CH:25]=[CH:26][C:9]([C:8]([F:7])([F:27])[F:28])=[CH:10][CH:11]=3)[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=3[CH2:18][CH2:17]2)=[O:44])[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1

参加物

5

反応物 3

HCID 7679Phenylacetyl chlorideHCID 8471TriethylamineHCID 14348987HCID 14348987、化合物

生成物 1

HCID 14348999HCID 14348999、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a cooled solution of 2,3,4,5-tetrahydro-1-(p-trifluoromethylphenoxy)-3-benzazepine of Example 1 (5.8 g. 0.019 mole) and triethylamine (2.3 g, 0.023 mole) in chloroform (75 ml) was slowly dropped phenylacetyl chloride (3.5 g. 0.023 mole) in chloroform (10 ml). After stirring at ambient temperature overnight the reaction mixture was concentrated to an oil. The oil was dissolved in ether, then washed with water, dilute HCl (10%), again with water and dried (saturated NaCl, anhydrous MgSO4). The solution was filtered, concentrated to an oil which was extracted with boiling hexanes and then concentrated to an oil (6.8 g, 84%). A sample was distilled to yield an oil of 3-phenylacetyl-2,3,4,5-tetrahydro-1-(p-trifluoromethylphenoxy)-3-benzazepine, 240°-250° C./0.1 mm.

後処理

  1. concentrationwas concentrated to an oil
  2. dissolutionThe oil was dissolved in ether
  3. washwashed with water, dilute HCl (10%), again with water
  4. dry with materialdried (saturated NaCl, anhydrous MgSO4)
  5. filtrationThe solution was filtered
  6. concentrationconcentrated to an oil which
  7. extractionwas extracted with boiling hexanes
  8. concentrationconcentrated to an oil (6.8 g, 84%)
  9. distillationA sample was distilled

出典と根拠

ORDレコード
ord-13887dbf179d449ea93bc1b81bd58793
出典データセット
uspto-grants-1991_10
特許番号
US05059688

反応ノート

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