Water → Ethyl 4-(2-Chlorodibenz[b,f][1,4]oxazepin-11-yl)-l-piperazineacetate

HRID 2225363

反応式

HRID 2225363 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[N:8]=[C:7]([N:16]3[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]3)[C:6]=2[CH:22]=1.Br[CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[N:8]=[C:7]([N:16]3[CH2:21][CH2:20][N:19]([CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26])[CH2:18][CH2:17]3)[C:6]=2[CH:22]=1

参加物

6

反応物 4

HCID 962WaterHCID 2170AmoxapineHCID 7748Ethyl bromoacetateHCID 11430Potassium Carbonate

生成物 1

HCID 15224710Ethyl 4-(2-Chlorodibenz[b,f][1,4]oxazepin-11-yl)-l-piperazineacetate収率 72%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 3.4 g of 2-chloro-11-(1-piperazinyl)dibenz[b,f][1,4]oxazepine, 2.00 g of ethyl bromoacetate and 1.38 g of potassium carbonate in 16 ml of N,N-dimethylformamide was stirred at 60°-70° C. for 3 hrs. After cooling, water was added to the reaction mixture and extracted with ether. The etheral layer was washed with water, dried and concentrated. The residue was chromatographed on silica gel using a mixture of n-hexane and ethyl acetate (2:1 and 1:1) as eluents to give 3.12 g of yellow crystals, which were recrystallized from n-hexane to give yellow prisms, mp 123°-123.5° C.

後処理

  1. temperatureAfter cooling
  2. extractionextracted with ether
  3. washThe etheral layer was washed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was chromatographed on silica gel using
  7. additiona mixture of n-hexane and ethyl acetate (2:1 and 1:1) as eluents

出典と根拠

ORDレコード
ord-8acf82bddd3b40eb9a38a3cc50e542c7
出典データセット
uspto-grants-1994_09
特許番号
US05344828

関連ノート

読み込み中…