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Sodium Hydroxide → HCID 57471196、化合物

HRID 1044492
ノート
印刷プレビュー

反応式

HRID 1044492 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:19]=[CH:20][C:21]=1[Cl:22])[CH2:5][CH:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([O:16]C)[CH:14]=2)[CH2:9][CH2:8][CH:7]1[NH2:18].[OH-].[Na+]>ClCCl>[NH2:18][CH:7]1[CH:6]([CH2:5][C:4]2[CH:19]=[CH:20][C:21]([Cl:22])=[C:2]([Cl:1])[CH:3]=2)[C:15]2[CH:14]=[C:13]([OH:16])[CH:12]=[CH:11][C:10]=2[CH2:9][CH2:8]1
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

4

反応物 2

HCID 14798Sodium HydroxideHCID 57467189HCID 57467189、化合物

生成物 1

HCID 57471196HCID 57471196、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
-10 °C

実験手順

1-(3,4-Dichlorobenzyl)-7-methoxy-1,2,3,4-tetrahydronaphthalen-2-amine (10 g, 26.8 mmol, cf. example 3.2 were dissolved in dichloromethane (240 mL). The suspension was cooled to −10° C. and a 1 M solution of bortribromide in dichloromethane (80 mL, 80 mmol). The solution was allowed to warm to room temperature and stirring was continued for 3 h. The reaction mixture was poured on ice (1 L). The aqueous layer was made alkaline (pH 10) with 2N sodium hydroxide solution. The layers were separated. The aqueous layer was extracted with dichloromethane and the combined organic layers were washed with saturated NaHCO3 solution and water. The organic layers were dried (Na2SO4) and concentrated in vacuo. The crude product was used without further purification for the next step. Yield: 10.8 g

後処理

  1. temperatureto warm to room temperature
  2. additionThe reaction mixture was poured on ice (1 L)
  3. customThe layers were separated
  4. extractionThe aqueous layer was extracted with dichloromethane
  5. washthe combined organic layers were washed with saturated NaHCO3 solution and water
  6. dry with materialThe organic layers were dried (Na2SO4)
  7. concentrationconcentrated in vacuo
  8. customThe crude product was used without further purification for the next step

出典と根拠

ORDレコード
ord-b156b9f320484ab281c55706bdd7f9a4
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08563617B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート