Diphenyl Ether → 3-(8-Chloro-dibenz[b,f][1,4]oxazepin-10(11H)-yl)-4-ethoxy-3-cyclobutene-1,2-dione

HRID 1707577

反応式

HRID 1707577 の反応式
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]2[O:6][C:7]3[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=3[CH:9]=[N:10][C:4]=2[CH:3]=1.[CH2:17]([O:19][C:20]1[C:21](=O)[C:22](=[O:27])[C:23]=1[O:24]CC)[CH3:18].C1(OC2C=CC=CC=2)C=CC=CC=1>O1CCOCC1>[Cl:1][C:2]1[CH:16]=[CH:15][C:5]2[O:6][C:7]3[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=3[CH2:9][N:10]([C:21]3[C:22](=[O:27])[C:23](=[O:24])[C:20]=3[O:19][CH2:17][CH3:18])[C:4]=2[CH:3]=1

参加物

5

反応物 3

HCID 7583Diphenyl EtherHCID 123228Diethyl squarateHCID 8382678-Chloro-dibenz[b,f]-[1,4]oxazepine

生成物 1

HCID 152322933-(8-Chloro-dibenz[b,f][1,4]oxazepin-10(11H)-yl)-4-ethoxy-3-cyclobutene-1,2-dione

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 8-chloro-dibenz[b,f][1,4]oxazepine (2 g), 3,4-diethoxy-3-cyclobutene-1,2-dione (5 g), diphenylether (2 g) and dioxane (10 mL) was heated to reflux. After 2 hours, most of the dioxane was removed in vacuo and the precipitated title compound (0.75 g) was collected by filtration as yellow solid. The filtrate was treated with cold methanol when more of the title compound (1.2 g) precipitated. This material was used in Example 6 without further purification.

後処理

  1. temperaturewas heated to reflux
  2. custommost of the dioxane was removed in vacuo
  3. customthe precipitated title compound (0.75 g)
  4. filtrationwas collected by filtration as yellow solid
  5. additionThe filtrate was treated with cold methanol when more of the title compound (1.2 g)
  6. customprecipitated
  7. customThis material was used in Example 6 without further purification

出典と根拠

ORDレコード
ord-57f9b35e48a04aa2872b5c7c2667e77f
出典データセット
uspto-grants-1994_10
特許番号
US05354746

関連ノート

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