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Ammonium Chloride → HCID 86748311、化合物

HRID 1492014
ノート
印刷プレビュー

反応式

HRID 1492014 の反応式
[Br-].[C:2]([CH2:6][CH2:7][CH2:8][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)([O:4][CH3:5])=[O:3].CC(C)([O-])C.[K+].[Si:34]([O:41][C@@H:42]1[CH2:46][O:45][C@H:44]([C:47]2[CH:48]=[N:49][CH:50]=[CH:51][CH:52]=2)[C@@H:43]1[CH2:53][CH2:54][CH:55]=O)([C:37]([CH3:40])([CH3:39])[CH3:38])([CH3:36])[CH3:35].[Cl-].[NH4+]>O1CCCC1.CCOCC>[Si:34]([O:41][C@@H:42]1[CH2:46][O:45][C@H:44]([C:47]2[CH:48]=[N:49][CH:50]=[CH:51][CH:52]=2)[C@@H:43]1[CH2:53][CH2:54]/[CH:55]=[CH:8]\[CH2:7][CH2:6][C:2]([O:4][CH3:5])=[O:3])([C:37]([CH3:40])([CH3:39])[CH3:38])([CH3:36])[CH3:35]
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 25517Ammonium ChlorideHCID 11015714(4-Methoxy-4-oxobutyl)triphenylphosphonium bromideHCID 18657617HCID 18657617、化合物HCID 23665647Potassium tert-butoxide

生成物 1

HCID 86748311HCID 86748311、化合物収率 69.7%

試薬・触媒・溶媒 2

HCID 3283
Diethyl Ether
溶媒
HCID 8028Tetrahydrofuran溶媒3 回

実験手順

To a suspension of 61.85 g (0.137 mol) of (3-carbomethoxy-1-propyl)triphenylphosphoniumbromide in 290 ml of tetrahydrofurane are added dropwise at 0° C. over argon with stirring, 116 ml (0.116 mol) of 1M solution of potassium tert-butoxide in tetrahydrofurane over a period of 20 min. The mixture is stirred at 0° C. for 1 h and a solution of 29.6 g of (2S,3S,4S)-3-[4-(t-butyldimethylsilyloxy)-2-(3-pyridyl)tetrahydrofuran-3-yl]propanal in 150 ml of tetrahydrofurane is added dropwise over a period of 15 min. The mixture is stirred at room temperature for an additional one h, 50 ml of concentrated aqueous ammonium chloride is added and the mixture is diluted with 2000 ml of ether. The mixture is washed with water and brine and the organic layer is dried (MgSO4) and evaporated. The residue is triturated with ether, the mixture is allowed to stand in the refrigerator overnight and the precipitated triphenylphosphine oxide is filtered and washed with ether. The combined filtrates are evaporated to dryness and the residue is subjected to flash chromatography on silica gel (5×30 cm2) using methylene chloride-ethyl acetate (1:1) as eluent to give 25.8 g of methyl (Z)-(2S,3S,4S)-7-[4-(t-butyldimethylsilyloxy)-2-(3-pyridyl)-tetrahydrofuran-3-yl]-4-heptenoate as an oil with elemental analysis: C,65.55; H,8.95; N,3.18 (theory: C,65.83; H,8.88; N,3.33) and optical rotation [α]D 25=+9.27 (methanol).

後処理

  1. additionare added dropwise at 0° C. over argon
  2. stirringThe mixture is stirred at 0° C. for 1 h
  3. additionis added
  4. washThe mixture is washed with water and brine
  5. dry with materialthe organic layer is dried (MgSO4)
  6. customevaporated
  7. customThe residue is triturated with ether
  8. customto stand in the refrigerator overnight
  9. filtrationthe precipitated triphenylphosphine oxide is filtered
  10. washwashed with ether
  11. customThe combined filtrates are evaporated to dryness

出典と根拠

ORDレコード
ord-22a95b6cc487455c92899a9eceb99019
出典データセット
uspto-grants-1994_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05371096

反応ノート

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