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Sodium Hydroxide → HCID 14990622、化合物

HRID 2248323
ノート
印刷プレビュー

反応式

HRID 2248323 の反応式
[OH-].[Na+].[OH:3][N:4]1[C:8]2[CH:9]=[C:10]([CH:13]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[OH:14])[CH:11]=[CH:12][C:7]=2[N:6]=[N:5]1>CO>[CH2:12]([O:3][N:4]1[C:8]2[CH:9]=[C:10]([CH:13]([C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=3)[OH:14])[CH:11]=[CH:12][C:7]=2[N:6]=[N:5]1)[CH2:7][CH2:8][CH3:9]
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

4

反応物 2

HCID 14798Sodium HydroxideHCID 149906211-hydroxy-alpha-phenyl-1H-benzotriazole-6-methanol

生成物 1

HCID 14990622HCID 14990622、化合物収率 87.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

To a stirred solution of 1.2 parts of sodium hydroxide in 40 parts of methanol were added 7.8 parts of 1-hydroxy-α-phenyl-1H-benzotriazole-6-methanol. After concentration, 18 parts of methylbenzene were added to the concentrate. The solvent was evaporated again and the residue was dissolved in 27 parts of N,N-dimethylformamide. 5.52 Parts of 1-iodobutane were added at once and the whole was stirred for 30 minutes at 50° C. After concentration, 30 parts of water were added. The solidified product was filtered off, washed with water and dissolved in dichloromethane. The organic layer was dried, filtered and evaporated. The residue was crystallized from 17.5 parts of 2,2'-oxybispropane. The product was filtered off and dried, yielding 7.8 parts (87.4%) of 1-butoxy-α-phenyl-1H-benzotriazole-6-methanol; mp. 89.2° C. (int. 65).

後処理

  1. concentrationAfter concentration, 18 parts of methylbenzene
  2. additionwere added to the concentrate
  3. customThe solvent was evaporated again
  4. dissolutionthe residue was dissolved in 27 parts of N,N-dimethylformamide
  5. addition5.52 Parts of 1-iodobutane were added at once and the whole
  6. concentrationAfter concentration, 30 parts of water
  7. additionwere added
  8. filtrationThe solidified product was filtered off
  9. washwashed with water
  10. dissolutiondissolved in dichloromethane
  11. customThe organic layer was dried
  12. filtrationfiltered
  13. customevaporated
  14. customThe residue was crystallized from 17.5 parts of 2,2'-oxybispropane
  15. filtrationThe product was filtered off
  16. customdried

出典と根拠

ORDレコード
ord-bb4ac646f36647838de69083f9b0d1f5
出典データセット
uspto-grants-1991_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05039677

反応ノート

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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