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Water → Ethyl 3-[4-(3-bromophenoxy)benzoyl]amino-4-cyclohexylaminobenzoate

HRID 1181312
ノート
印刷プレビュー

反応式

HRID 1181312 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:15]=[CH:16][CH:17]=1)[O:5][C:6]1[CH:14]=[CH:13][C:9]([C:10]([OH:12])=O)=[CH:8][CH:7]=1.[C:18](Cl)(=[O:22])[C:19](Cl)=O.C[N:25]([CH3:28])C=O.[OH2:29].C([N:32]([CH2:35][CH3:36])[CH2:33][CH3:34])C>C(Cl)(Cl)Cl>[Br:1][C:2]1[CH:3]=[C:4]([CH:15]=[CH:16][CH:17]=1)[O:5][C:6]1[CH:7]=[CH:8][C:9]([C:10]([NH:25][C:28]2[CH:8]=[C:9]([CH:10]=[CH:36][C:35]=2[NH:32][CH:33]2[CH2:34][CH2:16][CH2:17][CH2:2][CH2:3]2)[C:13]([O:22][CH2:18][CH3:19])=[O:29])=[O:12])=[CH:13][CH:14]=1
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 5

HCID 962WaterHCID 6228DimethylformamideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 219431614-(3-Bromophenoxy)benzoic acid

生成物 1

HCID 21943176Ethyl 3-[4-(3-bromophenoxy)benzoyl]amino-4-cyclohexylaminobenzoate収率 95%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

4-(3-Bromophenoxy)benzoic acid (74 g) was dissolved in chloroform (500 ml), and oxalyl chloride (33 ml) and dimethylformamide (catalytic amount) were added. The mixture was stirred for 4 hr at room temperature. The reaction mixture was concentrated under reduced pressure and dissolved in dichloromethane (150 ml). The resulting solution was added dropwise to a solution of ethyl 3-amino-4-cyclohexylaminobenzoate (66 g) obtained in the previous step in dichloromethane (500 ml) and triethylamine (71 ml), and the mixture was stirred for 1 hr at room temperature. The reaction mixture was poured into water and extracted with dichloromethane. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. Diethyl ether was added to the residue for crystallization and the crystals were collected by filtration to give the title compound (129 g, yield 95%).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. dissolutiondissolved in dichloromethane (150 ml)
  3. additionThe resulting solution was added dropwise to a solution of ethyl 3-amino-4-cyclohexylaminobenzoate (66 g)
  4. customobtained in the previous step in dichloromethane (500 ml)
  5. extractionextracted with dichloromethane
  6. washThe organic layer was washed with saturated brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. additionDiethyl ether was added to the residue for crystallization
  10. filtrationthe crystals were collected by filtration

出典と根拠

ORDレコード
ord-428dd3d11cc5409c918c2d706b95bcee
出典データセット
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07285551B2

反応ノート

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