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Sodium Hydroxide → 2-((2-(Aminomethyl)-3,5-dichlorobenzyl)oxy)ethanol

HRID 1481349
ノート
印刷プレビュー

反応式

HRID 1481349 の反応式
C([O:4][CH2:5][CH2:6][O:7][CH2:8][C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[C:11]([Cl:16])[C:10]=1[C:17]#[N:18])(=O)C.[OH-].[Na+]>C1COCC1.CO>[NH2:18][CH2:17][C:10]1[C:11]([Cl:16])=[CH:12][C:13]([Cl:15])=[CH:14][C:9]=1[CH2:8][O:7][CH2:6][CH2:5][OH:4]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 897048262-((3,5-Dichloro-2-cyanobenzyl)oxy)ethyl acetate

生成物 1

HCID 897049962-((2-(Aminomethyl)-3,5-dichlorobenzyl)oxy)ethanol

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

A solution of BH3 (1.46 mL, 1M in THF) was added to a solution of 2-((3,5-dichloro-2-cyanobenzyl)oxy)ethyl acetate (0.36 mmol) in 1.5 mL MeOH. The reaction mixture was heated to 60° C. for 3 h. At 0° C., 1.5 mL MeOH was dropwise added and the mixture was stirred until gaz evolution was finished. An aq. solution of 10% NaOH was added still under cooling. The solvent was removed under vacuo, the residue was diluted with water and extracted 3 times with EtOAc. The combined organic layers were dried over MgSO4 and concentrated in vacuo to give the desired product as yellow solid.

後処理

  1. temperatureunder cooling
  2. customThe solvent was removed under vacuo
  3. additionthe residue was diluted with water
  4. extractionextracted 3 times with EtOAc
  5. dry with materialThe combined organic layers were dried over MgSO4
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-b9cf52ed3a6946028814895c958f8ac9
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09409917B2

反応ノート

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