Sodium Chloride → HCID 21901780、化合物

HRID 719738ノート

反応式

HRID 719738 の反応式
S(Cl)(C)(=O)=O.[N+:6]([C:9]1[CH:14]=[CH:13][C:12]([N:15]2[CH2:19][CH2:18][CH2:17][CH:16]2[CH2:20]O)=[CH:11][CH:10]=1)([O-:8])=[O:7].C(N(CC)CC)C.[Cl-:29].[Na+]>CN(C=O)C>[Cl:29][CH2:20][CH:16]1[CH2:17][CH2:18][CH2:19][N:15]1[C:12]1[CH:13]=[CH:14][C:9]([N+:6]([O-:8])=[O:7])=[CH:10][CH:11]=1

参加物

6

反応物 4

HCID 5234Sodium ChlorideHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 6056432-Pyrrolidinemethanol, 1-(4-nitrophenyl)-

生成物 1

HCID 21901780HCID 21901780、化合物収率 882.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

27.9 ml (0.36 mol) of mesyl chloride were added dropwise to a solution of [1-(4-nitrophenyl)pyrrolidin-2-yl]methanol (66.7 g, 0.03 mol), 300 ml of anhydrous DMF and 58.5 ml (0.42 mol) of anhydrous triethylamine, cooled in an ice bath. The temperature was allowed to rise to 20° C. over one hour with stirring. 35.2 g (0.6 mol) of sodium chloride were added and the mixture was heated at 100° C. for one hour. The reaction medium was poured into 1.4 l of ice-water. The precipitate was filtered off, washed with water, dried and recrystallized from isopropanol. 63.7 g of a yellow powder (1) were thus obtained.

後処理

  1. temperaturecooled in an ice bath
  2. filtrationThe precipitate was filtered off
  3. washwashed with water
  4. customdried
  5. customrecrystallized from isopropanol

出典と根拠

ORDレコード
ord-db83a59d84f545d3a4a2b3b805ca0889
出典データセット
uspto-grants-2006_11
特許番号
US07132543B2

反応ノート

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