Triethylamine → HCID 70664766、化合物

HRID 1026626

反応式

HRID 1026626 の反応式
[Cl:1][C:2]1[C:7]2[CH2:8][CH:9]([C:10]([OH:12])=O)[C:6]=2[CH:5]=[CH:4][CH:3]=1.[CH2:13]([NH:20][CH2:21][C:22]([CH3:24])=[CH2:23])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.C(N(CC)CC)C.[O-]P1(OP([O-])(=O)OP([O-])(=O)OP([O-])(=O)O1)=O.[Na+].[Na+].[Na+].[Na+]>C(Cl)Cl>[CH2:13]([N:20]([CH2:21][C:22]([CH3:24])=[CH2:23])[C:10]([CH:9]1[C:6]2[CH:5]=[CH:4][CH:3]=[C:2]([Cl:1])[C:7]=2[CH2:8]1)=[O:12])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

参加物

6

反応物 4

HCID 8471TriethylamineHCID 25951Sodium tetrametaphosphate2 回HCID 102617682-Chlorobicyclo(4.2.0)octa-1(6),2,4-triene-7-carboxylic acidHCID 13788484N-Benzyl-2-methylprop-2-en-1-amine

生成物 1

HCID 70664766HCID 70664766、化合物収率 72%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 3-chloro-1,2-dihydrocyclobutabenzene-1-carboxylic acid (7.67 mmol, 1.4 g) in DCM (20 ml) was added N-benzyl-2-methylprop-2-en-1-amine (11.50 mmol, 1.854 g), triethylamine (15.33 mmol, 2.131 ml, 1.552 g) and cyclophos (50 wgt % solution in EtOAc) (9.20 mmol, 2.74 ml, 2.93 g). The mixture was stirred at ambient temperature overnight then cyclophos (50 wgt % solution in EtOAc) (0.5 ml) added and the mixture stirred for a further 1 hr. The mixture was diluted with DCM (10 ml), washed with 2 N HCl (20 ml) then 2 N NaOH (20 ml), dried over Na2SO4, filtered and concentrated under reduced pressure to afford N-benzyl-3-chloro-N-(2-methylallyl)-1,2-dihydrocyclobutabenzene-1-carboxamide as a brown oil (1.8 g).

後処理

  1. stirringthe mixture stirred for a further 1 hr
  2. washwashed with 2 N HCl (20 ml)
  3. dry with material2 N NaOH (20 ml), dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-4416d0814c924df4a2ef4dfd1f42386c
出典データセット
uspto-grants-2014_05
特許番号
US08729274B2

関連ノート

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