Triethylamine → Ethyl N-(4-chloro-2-pyrimidinyl)-N-methylglycinate

HRID 7632

反応式

HRID 7632 の反応式
Cl[C:2]1[N:7]=[C:6]([Cl:8])[CH:5]=[CH:4][N:3]=1.[CH3:9][NH:10][CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13].C(N(CC)CC)C>O1CCOCC1>[Cl:8][C:6]1[CH:5]=[CH:4][N:3]=[C:2]([N:10]([CH3:9])[CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])[N:7]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 775312,4-DichloropyrimidineHCID 95849Glycine, N-methyl-, ethyl ester

生成物 1

HCID 12056459Ethyl N-(4-chloro-2-pyrimidinyl)-N-methylglycinate

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

30.0 g (0.20 mol) of 2,4-dichloropyrimidine, 30.9 g (0.20 mol) of ethyl N-methylglycinate and 61.0 g (0.60 mol) of triethylamine in 200 ml of dioxane are stirred at 50° C. for 10 min. The mixture is filtered off with suction and the mother liquor is concentrated to half the original volume. A solid crystallizes out, which is filtered off with suction. The mother liquor is concentrated, the residue is stirred with petroleum ether and the product is filtered off.

後処理

  1. filtrationThe mixture is filtered off with suction
  2. concentrationthe mother liquor is concentrated to half the original volume
  3. customA solid crystallizes out, which
  4. filtrationis filtered off with suction
  5. concentrationThe mother liquor is concentrated
  6. filtrationthe product is filtered off

出典と根拠

ORDレコード
ord-8cdd1682398d44799c23b12882d311f3
出典データセット
uspto-grants-2006_08
特許番号
US07087616B2

関連ノート

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