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Sodium Iodide → N-[[1-[(2,3-dihydro-1,4-benzodioxin-2-yl)methyl]-4-piperidinyl]methyl]acetamide

HRID 1761498
ノート
印刷プレビュー

反応式

HRID 1761498 の反応式
Br[CH2:2][CH:3]1[O:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[O:5][CH2:4]1.C(O)(=O)C.[NH:17]1[CH2:22][CH2:21][CH:20]([CH2:23][NH:24][C:25](=[O:27])[CH3:26])[CH2:19][CH2:18]1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[Na+]>O.CN(C)C(=O)C>[O:8]1[C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[O:5][CH2:4][CH:3]1[CH2:2][N:17]1[CH2:22][CH2:21][CH:20]([CH2:23][NH:24][C:25](=[O:27])[CH3:26])[CH2:19][CH2:18]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 5238Sodium IodideHCID 10340Sodium CarbonateHCID 983332-Bromomethyl-1,4-benzodioxaneHCID 70352868N-(4-piperidinylmethyl)acetamide acetate

生成物 1

HCID 14049038N-[[1-[(2,3-dihydro-1,4-benzodioxin-2-yl)methyl]-4-piperidinyl]methyl]acetamide収率 21%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 31374Dimethylacetamide溶媒

反応条件

温度
75 °C

実験手順

A mixture of 12.6 parts of 2-(bromomethyl)-2,3-dihydro-1,4-benzodioxin, 11 parts of N-(4-piperidinylmethyl)acetamide acetate (1:1), 15 parts of sodium carbonate, 0.1 parts of sodium iodide and 135 parts of N,N-dimethylacetamide was stirred overnight at 75° C. The reaction mixture was poured into water. The product was extracted with 4-methyl-2-pentanone. The extract was dried, filtered and evaporated. The residue was crystallized from a mixture of 1,1'-oxybisethane and 2,2'-oxybispropane. The product was filtered off and dried, yielding 3.2 parts (21.0%) of N-[[1-[(2,3-dihydro-1,4-benzodioxin-2-yl)methyl]-4-piperidinyl]methyl]acetamide; mp. 137.9° C. (intermediate 89).

後処理

  1. extractionThe product was extracted with 4-methyl-2-pentanone
  2. customThe extract was dried
  3. filtrationfiltered
  4. customevaporated
  5. customThe residue was crystallized from a mixture of 1,1'-oxybisethane and 2,2'-oxybispropane
  6. filtrationThe product was filtered off
  7. customdried

出典と根拠

ORDレコード
ord-9d927ba85736464ba10e9ab6684ab661
出典データセット
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04826848

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート