Thionyl Chloride → 2-[(3-Chloro-2-chloromethyl-pyridin-4-yl)-methyl-amino]-ethanol

HRID 1637622ノート

反応式

HRID 1637622 の反応式
S(Cl)([Cl:3])=O.[Cl:5][C:6]1[C:7]([CH2:17]O)=[N:8][CH:9]=[CH:10][C:11]=1[N:12]([CH3:16])[CH2:13][CH2:14][OH:15]>ClCCl>[Cl:5][C:6]1[C:7]([CH2:17][Cl:3])=[N:8][CH:9]=[CH:10][C:11]=1[N:12]([CH3:16])[CH2:13][CH2:14][OH:15]

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 537528042-[(3-Chloro-2-hydroxymethyl-pyridin-4-yl)-methylamino]-ethanol

生成物 1

HCID 543658082-[(3-Chloro-2-chloromethyl-pyridin-4-yl)-methyl-amino]-ethanol

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Thionyl chloride (7.4 ml, 101.5 mmol), dissolved in dichloromethane (50 ml), is added dropwise at 4° C. to a solution of (2-[(3-chloro-2-hydroxymethyl-pyridin-4-yl)-methylamino]-ethanol (10.0 g, 46.1 mmol) in dichloromethane (150 ml). The solution is stirred for 1 h at this temperature, triturated with ice water and neutralized with saturated sodium bicarbonate solution. After separation of the organic layer the aqueous phase is extracted with dichloromethane. The combined organic extracts are washed with water, dried over magnesium sulfate and evaporated in vacuo. The residue is employed without additional purification for the synthesis described in step b).

後処理

  1. customtriturated with ice water and neutralized with saturated sodium bicarbonate solution
  2. customAfter separation of the organic layer the aqueous phase
  3. extractionis extracted with dichloromethane
  4. washThe combined organic extracts are washed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated in vacuo
  7. customThe residue is employed without additional purification for the synthesis

出典と根拠

ORDレコード
ord-9ac5451a145a4c1aa3d52696820f22b5
出典データセット
uspto-grants-2000_03
特許番号
US06043242

反応ノート

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