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

HRID 1587478

反応式

HRID 1587478 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 40%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

To a solution of 5g (17.7mmol) of 1-n-dodecylazacycloheptan-2-one in 150ml of benzene was added 4.18g (9.4mmol) 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.llg (40%) of 1-n-dodecylazacycloheptane-2-thione.

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-502ff0342b0a44e6b0a104d39a13916c
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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