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4-Chlorobenzoyl chloride → 4-Chloro-N-[[2-[2-(4-morpholinyl)ethoxy]phenyl]methyl]-N-(2-phenylethyl)benzamide, hydrochloride salt

HRID 26968
ノート
印刷プレビュー

反応式

HRID 26968 の反応式
[N:1]1([CH2:7][CH2:8][O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[CH2:16][NH:17][CH2:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[Cl:26][C:27]1[CH:35]=[CH:34][C:30]([C:31](Cl)=[O:32])=[CH:29][CH:28]=1>C(Cl)(Cl)Cl.CCOCC>[ClH:26].[Cl:26][C:27]1[CH:35]=[CH:34][C:30]([C:31]([N:17]([CH2:16][C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[O:9][CH2:8][CH2:7][N:1]2[CH2:2][CH2:3][O:4][CH2:5][CH2:6]2)[CH2:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:32])=[CH:29][CH:28]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 85014-Chlorobenzoyl chlorideHCID 21322749N-[[2-[2-(4-Morpholinyl)ethoxy]phenyl]methyl]benzeneethanamine

生成物 1

HCID 1317113154-Chloro-N-[[2-[2-(4-morpholinyl)ethoxy]phenyl]methyl]-N-(2-phenylethyl)benzamide, hydrochloride salt収率 168.8%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6212Chloroform溶媒

実験手順

N-[[2-[2-(4-Morpholinyl)ethoxy]phenyl]methyl]benzeneethanamine (40 g) and 22 g of p-chlorobenzoyl chloride are reacted in 600 ml of chloroform following the procedure described in Example 1C. The residue from the chloroform evaporation is first triturated with ether (evaporation repeated) and then with 400 ml of warm acetone to give a crystalline product. After diluting with 500 ml of ether and cooling for about 16 hours, the solid is filtered under nitrogen, washed with ether and dried in vacuo to yield 54.7 g of material, melting point 147°-149° C. (sintering at 145° C.). Crystallization from 250 ml of warm methanol-1750 ml ether yield 52.9 g of the title compound, melting point 147°-149° C.

後処理

  1. customThe residue from the chloroform evaporation
  2. customis first triturated with ether (evaporation repeated)
  3. customwith 400 ml of warm acetone to give a crystalline product
  4. temperaturecooling for about 16 hours
  5. filtrationthe solid is filtered under nitrogen
  6. washwashed with ether
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-ef7f1125e2584476ae7a2f558029ebd1
出典データセット
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04151354

反応ノート

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