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Thionyl Chloride → N-(4-chloromethylphenyl)-7-(4-methylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide

HRID 566040
ノート
印刷プレビュー

反応式

HRID 566040 の反応式
O[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]([C:12]2[CH2:13][CH2:14][O:15][C:16]3[CH:22]=[CH:21][C:20]([C:23]4[CH:28]=[CH:27][C:26]([CH3:29])=[CH:25][CH:24]=4)=[CH:19][C:17]=3[CH:18]=2)=[O:11])=[CH:5][CH:4]=1.S(Cl)([Cl:32])=O>N1C=CC=CC=1.C(Cl)(Cl)Cl.O>[Cl:32][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]([C:12]2[CH2:13][CH2:14][O:15][C:16]3[CH:22]=[CH:21][C:20]([C:23]4[CH:28]=[CH:27][C:26]([CH3:29])=[CH:25][CH:24]=4)=[CH:19][C:17]=3[CH:18]=2)=[O:11])=[CH:5][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 24386Thionyl ChlorideHCID 18472380N-(4-hydroxymethylphenyl)-7-(4-methylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide

生成物 1

HCID 18472316N-(4-chloromethylphenyl)-7-(4-methylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide収率 88%

試薬・触媒・溶媒 3

HCID 1049Pyridine触媒HCID 962Water溶媒
HCID 6212
Chloroform
溶媒

実験手順

To a solution of N-(4-hydroxymethylphenyl)-7-(4-methylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide (412 mg, 1.07 mmol) and pyridine (1 drop) in chloroform (5 ml) was dropwise added thionyl chloride (0.14 ml, 1.61 mmol), and the mixture was stirred for 2 hours. The mixture was diluted with water and extracted with chloroform. The extract was washed with saturated sodium chloride solution and dried with magnesium sulfate. The solvent was evaporated, and the resulting powder was washed with hexane-ethyl acetate (1:1) to give N-(4-chloromethylphenyl)-7-(4-methylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide (380 mg, 88%) as colorless powder.

後処理

  1. extractionextracted with chloroform
  2. washThe extract was washed with saturated sodium chloride solution
  3. dry with materialdried with magnesium sulfate
  4. customThe solvent was evaporated
  5. washthe resulting powder was washed with hexane-ethyl acetate (1:1)

出典と根拠

ORDレコード
ord-dddfa8020ad14539bb9a1319ba5ef1b7
出典データセット
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06172061B2

反応ノート

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