Iodoethane → HCID 67205011、化合物

HRID 1894318ノート

反応式

HRID 1894318 の反応式
[CH2:1]([O:3][C:4](=[O:16])[C:5]1[C:10]([OH:11])=[CH:9][C:8]([C:12]([CH3:15])([CH3:14])[CH3:13])=[N:7][CH:6]=1)[CH3:2].C(=O)([O-])[O-].[K+].[K+].[CH2:23](I)[CH3:24]>CN(C)C=O.O.[Cl-].[Na+].O>[CH2:1]([O:3][C:4](=[O:16])[C:5]1[C:10]([O:11][CH2:23][CH3:24])=[CH:9][C:8]([C:12]([CH3:15])([CH3:14])[CH3:13])=[N:7][CH:6]=1)[CH3:2]

参加物

7

反応物 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 178469765HCID 178469765、化合物

生成物 1

HCID 67205011HCID 67205011、化合物収率 80%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

6-tert-Butyl-4-hydroxy-nicotinic acid ethyl ester (110 mg, 0.5 mmol) was dissolved in dimethylformamide (6 mL). Potassium carbonate was added followed by dropwise addition of ethyl iodine (0.13 mL, 1.5 mmol). The reaction mixture was stirred at room temperature overnight. It was diluted with water and brine and extracted with diethyl ether (2×30 mL). Combined organics washed with brine/water, dried and concentrated to give 6-tert-butyl-4-ethoxy-nicotinic acid ethyl ester as viscous oil (100 mg, 80%). LR-MS: 251 [(M+H)+]

後処理

  1. extractionextracted with diethyl ether (2×30 mL)
  2. washCombined organics washed with brine/water
  3. customdried
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-2607a40e64bd4ba6b10ccc5724155844
出典データセット
uspto-grants-2013_08
特許番号
US08513239B2

反応ノート

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