Phosphorus sulfide (P2S5) → N-dodecylazepan-2-thione

HRID 1656893ノート

反応式

HRID 1656893 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].P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:22]>C1C=CC=CC=1>[CH2:1]([N:13]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][C:14]1=[S:22])[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

4

反応物 2

HCID 14817Phosphorus sulfide (P2S5)HCID 42981Laurocapram

生成物 1

HCID 10108679N-dodecylazepan-2-thione収率 75.4%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

To a solution of 5 g (17.7 mmol) of 1-n-dodecylazacycloheptan-2-one in 150 ml of benzene was added 4.18 g (9.4 mmol) of phosphorus pentasulfide and the mixture was refluxed for 1 hr. After cooling to room temperature, the mixture was filtered and the solid was washed with chloroform and ethanol. The filtrate was concentrated in vacuo and the residue was subjected to flash chromatography, (silica; (95:5)V/V hexane/ethyl acetate) to give 2.11 g (40%) of 1-n-dodecylazacycloheptane-2thione.

後処理

  1. temperaturethe mixture was refluxed for 1 hr
  2. filtrationthe mixture was filtered
  3. washthe solid was washed with chloroform and ethanol
  4. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-62f2298416ec4fd398b32b404b3188d3
出典データセット
uspto-grants-1993_10
特許番号
US05256647

反応ノート

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