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Benzyl Bromide → HCID 69334435、化合物

HRID 1003189
ノート
印刷プレビュー

反応式

HRID 1003189 の反応式
[OH:1][C:2]1[C:19]([N+:20]([O-:22])=[O:21])=[CH:18][C:17]2[C@@H:16]3[C@H:7]([C@H:8]4[C@@:12]([CH2:14][CH2:15]3)([CH3:13])[C:11](=[O:23])[CH2:10][CH2:9]4)[CH2:6][CH2:5][C:4]=2[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:30](Br)[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1.[NH4+].[Cl-]>CN(C=O)C>[CH2:30]([O:1][C:2]1[C:19]([N+:20]([O-:22])=[O:21])=[CH:18][C:17]2[C@@H:16]3[C@H:7]([C@H:8]4[C@@:12]([CH2:14][CH2:15]3)([CH3:13])[C:11](=[O:23])[CH2:10][CH2:9]4)[CH2:6][CH2:5][C:4]=2[CH:3]=1)[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 25517Ammonium ChlorideHCID 2334963-Hydroxy-2-nitroestra-1,3,5(10)-trien-17-one

生成物 1

HCID 69334435HCID 69334435、化合物収率 99.1%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

To a solution of 3-hydroxy-2-nitroestra-1,3,5(10)-trien-17-one (76b, 1.58 g, 5.0 mmol) in DMF (20 mL) were added potassium carbonate (1.38 g, 10 mmol) and benzyl bromide (0.9 mL, 7.5 mmol) and stirred for 19 h at room temperature. To the reaction mixture was added saturated aqueous NH4Cl at 0° C. and extracted with CHCl3. The combined organic layers were washed with H2O, saturated aqueous NaCl, and then dried (Na2SO4). The desiccant was filtered and the solvent was evaporated at reduced pressure. The residue was washed with Et2O to afford 2.01 g of 79 (99% yield) mp: 234-235° C.

後処理

  1. extractionextracted with CHCl3
  2. washThe combined organic layers were washed with H2O, saturated aqueous NaCl
  3. dry with materialdried (Na2SO4)
  4. filtrationThe desiccant was filtered
  5. customthe solvent was evaporated at reduced pressure
  6. washThe residue was washed with Et2O

出典と根拠

ORDレコード
ord-6a13a30ca65b420c87bf8d45ddb81421
出典データセット
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06046186

反応ノート

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