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Water → 5-Chloro-3-[2-tritylamino-3-(1-trityl-4-imidazolyl)propoxy]-1,2-benzoisoxazole

HRID 1901641
ノート
印刷プレビュー

反応式

HRID 1901641 の反応式
[C:1]([NH:20][CH:21]([CH2:24][C:25]1[N:26]=[CH:27][N:28]([C:30]([C:43]2[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=2)([C:37]2[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=2)[C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[CH:29]=1)[CH2:22][OH:23])([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+].Cl[C:52]1[C:56]2[CH:57]=[C:58]([Cl:61])[CH:59]=[CH:60][C:55]=2[O:54][N:53]=1.O>CN(C)C=O.C(OCC)(=O)C>[Cl:61][C:58]1[CH:59]=[CH:60][C:55]2[O:54][N:53]=[C:52]([O:23][CH2:22][CH:21]([NH:20][C:1]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)([C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=3)[CH2:24][C:25]3[N:26]=[CH:27][N:28]([C:30]([C:43]4[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=4)([C:37]4[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=4)[C:31]4[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=4)[CH:29]=3)[C:56]=2[CH:57]=1
参加物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 962WaterHCID 24758Sodium hydrideHCID 135684483,5-Dichloro-1,2-benzoxazoleHCID 233684162-Tritylamino-3-(1-trityl-4-imidazolyl)-1-propanol

生成物 1

HCID 233683685-Chloro-3-[2-tritylamino-3-(1-trityl-4-imidazolyl)propoxy]-1,2-benzoisoxazole

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
3 回
HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 2.0 g of 2-tritylamino-3-(1-trityl-4-imidazolyl)-1-propanol in 10 ml of N,N-dimethylformamide is dropwise added to a suspension of 0.14 g of 60% (w/w) sodium hydride in 15 ml of N,N-dimethylformamide at room temperature over 15 minutes, and the temperature is then elevated gradually to 80° C., after which this is added to a solution of 0.6 g of 3,5-dichloro-1,2-benzoisoxazole in 10 ml of N,N-dimethylformamide. They are subjected to reaction at the same temperature for six hours. After cooling, water and ethyl acetate are added and shaken, and the organic layer is separated. The separated organic layer is washed with a saturated saline solution and dried over anhydrous magnesium sulfate, after which the solvent is removed by distillation under reduced pressure. The residue obtained is purified by a column chromatography [eluant:n-hexane:ethyl acetate=3:1], to obtain 1.12 g of colorless, crystalline 5-chloro-3-[2-tritylamino-3-(1-trityl-4-imidazolyl)propoxy]-1,2-benzoisoxazole having a melting point of 113.4°-114.7° C.

後処理

  1. customis then elevated gradually to 80° C.
  2. customThey are subjected to reaction at the same temperature for six hours
  3. temperatureAfter cooling
  4. customthe organic layer is separated
  5. washThe separated organic layer is washed with a saturated saline solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customafter which the solvent is removed by distillation under reduced pressure
  8. customThe residue obtained
  9. customis purified by a column chromatography [eluant:n-hexane:ethyl acetate=3:1]

出典と根拠

ORDレコード
ord-bf166d6133e749fdac8664feb9566c8e
出典データセット
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05578627

反応ノート

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