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Triethylamine → 4-chloro-3-methoxy-N-(4-methyl-1,2,5-oxadiazol-3-yl)-2,3-dihydro-1-benzothiophene-5-carboxamide 1,1-dioxide

HRID 575915
ノート
印刷プレビュー

反応式

HRID 575915 の反応式
[Cl:1][C:2]1[C:7]2[CH:8]([O:13][CH3:14])[CH2:9][S:10](=[O:12])(=[O:11])[C:6]=2[CH:5]=[CH:4][C:3]=1[C:15]([OH:17])=O.[CH3:18][C:19]1[C:20]([NH2:24])=[N:21][O:22][N:23]=1.C(P1(=O)OP(=O)(CCC)OP(=O)(CCC)O1)CC.C(N(CC)CC)C>C(Cl)Cl.CN(C)C1C=CN=CC=1>[Cl:1][C:2]1[C:7]2[CH:8]([O:13][CH3:14])[CH2:9][S:10](=[O:11])(=[O:12])[C:6]=2[CH:5]=[CH:4][C:3]=1[C:15]([NH:24][C:20]1[C:19]([CH3:18])=[N:23][O:22][N:21]=1)=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 286743-Amino-4-methylfurazanHCID 111923Propylphosphonic anhydrideHCID 867154224-Chloro-3-methoxy-2,3-dihydro-1-benzothiophene-5-carboxylic acid 1,1-dioxide

生成物 1

HCID 867154214-chloro-3-methoxy-N-(4-methyl-1,2,5-oxadiazol-3-yl)-2,3-dihydro-1-benzothiophene-5-carboxamide 1,1-dioxide

試薬・触媒・溶媒 2

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 6344Dichloromethane溶媒

実験手順

1.00 g (3.14 mmol) of 4-chloro-3-methoxy-2,3-dihydro-1-benzothiophene-5-carboxylic acid 1,1-dioxide and 0.33 g (3.15 mmol) of 4-methyl-1,2,5-oxadiazol-3-yl-amine were dissolved at room temperature (RT) in 35 ml of CH2Cl2, 3.02 g (4.74 mmol) of 2,4,6-tripropyl-1,3,5,2,4,6-trioxatriphosphinane 2,4,6-trioxide (50% solution in THF) were added and the mixture was stirred at RT for 1 h. Subsequently, 2.18 ml (15.64 mmol) of triethylamine and 75 mg (0.61 mmol) of 4-dimethylaminopyridine (DMAP) were added and the whole mixture was stirred at RT for 16 h. This was followed by washing with water and twice with 6N hydrochloric acid, drying of the organic phase over Na2SO4 and filtration with suction through silica gel, washing through with 1:2 heptane/ethyl acetate and concentration. Yield 708 mg (63%).

後処理

  1. stirringthe whole mixture was stirred at RT for 16 h
  2. washby washing with water and twice with 6N hydrochloric acid
  3. dry with materialdrying of the organic phase over Na2SO4 and filtration with suction through silica gel
  4. washwashing through with 1:2 heptane/ethyl acetate and concentration

出典と根拠

ORDレコード
ord-17834b21d09d441f81d075bdb2ca113d
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09035067B2

反応ノート

読み込み中…

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