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

HRID 1637622노트

반응식

HRID 1637622 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9ac5451a145a4c1aa3d52696820f22b5
출처 데이터셋
uspto-grants-2000_03
특허 번호
US06043242

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