Hydrochloric Acid → Dibenz(c,e)oxepin-5(7H)-one

HRID 2109531

反応式

HRID 2109531 の反応式
[BH4-].[Na+].[C:3]12[C:10]3=[CH:11][CH:12]=[CH:13][CH:14]=[C:9]3[C:8](=O)[O:7][C:5](=[O:6])[C:4]1=[CH:16][CH:17]=[CH:18][CH:19]=2.Cl>CN(C=O)C.O>[CH:19]1[C:3]2[C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=3[CH2:8][O:7][C:5](=[O:6])[C:4]=2[CH:16]=[CH:17][CH:18]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 72794Diphenic anhydrideHCID 4311764Sodium borohydride

生成物 1

HCID 4613402Dibenz(c,e)oxepin-5(7H)-one収率 75.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

9.0 g (0.24 mol) of sodium borohydride were added in portions at 5° C. in the course of 10 min to a suspension of 50.0 g (0.22 mol) of diphenic anhydride in 220 ml of DMF. After stirring at RT for 1 h, the reaction mixture was poured onto 220 ml of 6 M hydrochloric acid, diluted with 750 ml of water and stirred for 2 h. The deposited precipitate was filtered off with suction and 35.0 g of 7H-dibenzo[c,e]oxepin-5-one were obtained; m.p. 131° C.

後処理

  1. stirringstirred for 2 h
  2. filtrationThe deposited precipitate was filtered off with suction

出典と根拠

ORDレコード
ord-9bed43b74d8d40dcb5a68ff0bb463461
出典データセット
uspto-grants-2009_04
特許番号
US07514582B2

関連ノート

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