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Ammonium Chloride → 1alpha,3beta-Bis(tert-butyldimethylsilyloxy)-17beta-{4-ethyl-4-(triethylsilyloxy)hexyloxymethyl}androst-5-ene

HRID 1792228
ノート
印刷プレビュー

反応式

HRID 1792228 の反応式
[Si:1]([O:8][C@@H:9]1[C@@:26]2([CH3:27])[C:13](=[CH:14][CH2:15][C@@H:16]3[C@@H:25]2[CH2:24][CH2:23][C@@:21]2([CH3:22])[C@H:17]3[CH2:18][CH2:19][C@@H:20]2[CH2:28][OH:29])[CH2:12][C@@H:11]([O:30][Si:31]([C:34]([CH3:37])([CH3:36])[CH3:35])([CH3:33])[CH3:32])[CH2:10]1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[H-].[K+].C1OCCOCCOCCOCCOCCOC1.Br[CH2:59][CH2:60][CH2:61][C:62]([CH2:73][CH3:74])([O:65][Si:66]([CH2:71][CH3:72])([CH2:69][CH3:70])[CH2:67][CH3:68])[CH2:63][CH3:64].[Cl-].[NH4+]>O1CCCC1>[Si:1]([O:8][C@@H:9]1[C@@:26]2([CH3:27])[C:13](=[CH:14][CH2:15][C@@H:16]3[C@@H:25]2[CH2:24][CH2:23][C@@:21]2([CH3:22])[C@H:17]3[CH2:18][CH2:19][C@@H:20]2[CH2:28][O:29][CH2:59][CH2:60][CH2:61][C:62]([CH2:73][CH3:74])([O:65][Si:66]([CH2:71][CH3:72])([CH2:67][CH3:68])[CH2:69][CH3:70])[CH2:63][CH3:64])[CH2:12][C@@H:11]([O:30][Si:31]([C:34]([CH3:37])([CH3:36])[CH3:35])([CH3:32])[CH3:33])[CH2:10]1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]
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 5

HCID 25517Ammonium ChlorideHCID 2855718-Crown-6HCID 82127Potassium hydrideHCID 220276701-Bromo-4-ethyl-4-(triethylsilyloxy)hexaneHCID 696299821alpha,3beta-Bis(tert-butyldimethylsilyloxy)-17beta-(hydroxymethyl)androst-5-ene

生成物 1

HCID 69630124
1alpha,3beta-Bis(tert-butyldimethylsilyloxy)-17beta-{4-ethyl-4-(triethylsilyloxy)hexyloxymethyl}androst-5-ene
収率 99.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

1α,3β-Bis(tert-butyldimethylsilyloxy)-17β-(hydroxymethyl)androst-5-ene (11.0 g) was dissolved in tetrahydrofuran. Under cooling with ice, potassium hydride (30% in oil, 200.3 g) and 18-crown-6 (2.64 g) were added to the solution, which was then stirred for 5 min. 1-Bromo-4-ethyl-4-(triethylsilyloxy)hexane (25.91 g) was then added to the mixture and reacted for 3.5 hours. After stopping the reaction by adding a saturated aqueous ammonium chloride solution, the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, filtered and the filtrate was evaporated under reduced pressure to remove the solvent. The resulting residue was purified by column chromatography (hexane:ethyl acetate=50:1) to give the titled compound (15.8 g).

後処理

  1. additionwere added to the solution, which
  2. customreacted for 3.5 hours
  3. customthe reaction
  4. extractionthe mixture was extracted with ethyl acetate
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customthe filtrate was evaporated under reduced pressure
  8. customto remove the solvent
  9. customThe resulting residue was purified by column chromatography (hexane:ethyl acetate=50:1)

出典と根拠

ORDレコード
ord-851c9b370e384106b3146c8a63abe960
出典データセット
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07074777B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート