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Diethyl Ether → HCID 20688053、化合物

HRID 1596816
ノート
印刷プレビュー

反応式

HRID 1596816 の反応式
[CH:1]#[C:2][CH2:3][CH2:4][CH3:5].C([Li])CCC.[C:11]([C:15]1([C:18]([CH3:21])([CH3:20])[CH3:19])[CH2:17][O:16]1)([CH3:14])([CH3:13])[CH3:12].C(OCC)C>CCCCC.CN(P(N(C)C)(N(C)C)=O)C>[C:11]([C:15]([OH:16])([CH2:17][C:1]#[C:2][CH2:3][CH2:4][CH3:5])[C:18]([CH3:21])([CH3:20])[CH3:19])([CH3:14])([CH3:13])[CH3:12]
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 3283Diethyl EtherHCID 123091-PentyneHCID 3293992,2-ditert-butyloxiraneHCID 178418339Butyllithium

生成物 1

HCID 20688053HCID 20688053、化合物収率 84.3%

試薬・触媒・溶媒 2

HCID 8003Pentane溶媒
HCID 12679
Hexamethylphosphoramide
溶媒
2 回

実験手順

1.26 ml (12.8 mmol) 1-pentyne were added dropwise at 0° C. under argon for 5 minutes to 8.0 ml (12.8 mmol) of a 1.6-molar n-butyllithium solution in pentane. The solution obtained was cooled for another 15 minutes, and then the solvent was withdrawn under reduced pressure. 5 ml HMPA and a solution of 1.0 g (6.4 mmol) 2,2-di-tert-butyloxirane in 2 ml HMPA were added. The reaction solution was stirred for 20 hours at room temperature. Subsequently, it was processed analogous to Example 1. The raw product obtained was cleaned by means of a silica column with 2% diethyl ether/light gasoline. There were obtained 1.21 g (84%) 3-tert-butyl-2,2-dimethylnon-5-in-3-ol

後処理

  1. customThe solution obtained
  2. temperaturewas cooled for another 15 minutes
  3. customthe solvent was withdrawn under reduced pressure
  4. customThe raw product obtained

出典と根拠

ORDレコード
ord-078e20830dac494285372dda7a6ff218
出典データセット
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06291713B1

反応ノート

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