Sodium Sulfate → 1-Dodecylazepane

HRID 1587477

反応式

HRID 1587477 の反応式
[CH2:1]([N:13]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][C:14]1=O)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].[H-].[Al+3].[Li+].[H-].[H-].[H-].S([O-])([O-])(=O)=O.[Na+].[Na+]>C(OCC)C>[CH2:1]([N:13]1[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19]1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]

参加物

5

反応物 3

HCID 24436Sodium SulfateHCID 42981LaurocapramHCID 21226445Aluminium lithium hydride

生成物 1

HCID 33661291-Dodecylazepane収率 93.5%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

56.2g (0.2 mol) of 1-dodecylazacycloheptan-2-one in 100ml diethyl ether was added dropwise to a suspension of 7.6g (0.2 mol) lithium aluminum hydride in 100ml diethyl ether under argon at room temperature. After 5 hours of stirring, 20ml saturated sodium sulfate was added dropwise. The mixture was filtered and the filtrate was dried with magnesium sulfate, filtered and concentrated. The resulting oil was distilled (130°/.03 mm) to yield 50.03g (93.5%) of 1-n-dodecylazacycloheptane.

後処理

  1. filtrationThe mixture was filtered
  2. dry with materialthe filtrate was dried with magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. distillationThe resulting oil was distilled (130°/.03 mm)

出典と根拠

ORDレコード
ord-124f3113283747acbf5f492760bd94d0
出典データセット
uspto-grants-1993_06
特許番号
US05218113

関連ノート

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