Chloromethyl benzoate → HCID 13881954、化合物

HRID 543160

反応式

HRID 543160 の反応式
[CH3:1][N:2]([CH3:12])[C:3]([O:5][C:6]1[CH:7]=[N:8][CH:9]=[CH:10][CH:11]=1)=[O:4].[Cl:13][CH2:14][O:15][C:16](=[O:23])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>C(OCC)C>[Cl-:13].[CH3:1][N:2]([CH3:12])[C:3]([O:5][C:6]1[CH:7]=[N+:8]([CH2:14][O:15][C:16]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[O:23])[CH:9]=[CH:10][CH:11]=1)=[O:4]

参加物

4

反応物 2

HCID 79257Chloromethyl benzoateHCID 98821Norpyridostigmine

生成物 1

HCID 13881954HCID 13881954、化合物収率 85.2%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

3-Dimethylcarbamoyloxypyridine (4.98 g) and chloromethylbenzoate (5.13 g) were heated to 70° C. with stirring for 4 hrs. The hot reaction mixture was poured into 100 ml of diethyl ether with vigorous stirring. The precipitated solids were filtered off and washed twice with anhydrous diethyl ether (100 ml×2). Recrystallization from acetone gave 8.6 g of 3-(dimethylcarbamoyloxy)-1-(phenylcarbonyloxymethyl)pyridinium chloride as prisms, m.p. 175°-176° C.

後処理

  1. filtrationThe precipitated solids were filtered off
  2. washwashed twice with anhydrous diethyl ether (100 ml×2)
  3. customRecrystallization from acetone

出典と根拠

ORDレコード
ord-4fe42735981d4326ac1d16bf7b548e47
出典データセット
uspto-grants-1987_04
特許番号
US04661502

関連ノート

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