1,2-Dichloroethane → HCID 22135199、化合物

HRID 491008ノート

反応式

HRID 491008 の反応式
[CH3:1][O:2][C:3]([C:5]1([C:10]([OH:12])=O)[CH2:9][CH2:8][CH2:7][CH2:6]1)=[O:4].C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl.[CH3:27][CH:28]([CH3:32])[CH2:29][CH2:30][NH2:31]>C(Cl)Cl.CN(C=O)C.O>[CH3:27][CH:28]([CH3:32])[CH2:29][CH2:30][NH:31][C:10]([C:5]1([C:3]([O:2][CH3:1])=[O:4])[CH2:6][CH2:7][CH2:8][CH2:9]1)=[O:12]

参加物

7

反応物 4

HCID 111,2-DichloroethaneHCID 7894IsoamylamineHCID 757711-HydroxybenzotriazoleHCID 18317887HCID 18317887、化合物

生成物 1

HCID 22135199HCID 22135199、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 22350042dichloromethane N,N-dimethylformamide溶媒

実験手順

To 1-(methoxycarbonyl)cyclopentanecarboxylic acid (630 mg, 3.7 mmol) in CH2Cl2/DMF (5:1, 37 mL) at 0° C. was added HOBT (730 mg, 4.8 mmol) and EDC (920 mg, 4.8 mmol). The mixture was stirred for 10 min then 3-methylbutylamine (640 mg, 7.4 mmol) was added and stirring was continued for 1 h. The solution was poured into water and the layers separated. The aqueous layer was extracted with methylene chloride and the combined extracts were washed with water, 1N HCl, sat'd NaHCO3, dried over magnesium sulfate, and concentrated to a glassy solid (800 mg, 90%). MS [M+H]+ 243.

後処理

  1. stirringstirring
  2. waitwas continued for 1 h
  3. customthe layers separated
  4. extractionThe aqueous layer was extracted with methylene chloride
  5. washthe combined extracts were washed with water, 1N HCl
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated to a glassy solid (800 mg, 90%)

出典と根拠

ORDレコード
ord-d468ca36fbd7492190071cc3fbe5e8f8
出典データセット
uspto-grants-2009_05
特許番号
US07528249B2

反応ノート

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