Water → Diethyl 4-isothiocyanatobenzylphosphonate

HRID 25512

反応式

HRID 25512 の反応式
[C:1](Cl)(Cl)=[S:2].[NH2:5][C:6]1[CH:20]=[CH:19][C:9]([CH2:10][P:11](=[O:18])([O:15][CH2:16][CH3:17])[O:12][CH2:13][CH3:14])=[CH:8][CH:7]=1.C(=O)(O)[O-].[Na+].O>ClCCl>[N:5]([C:6]1[CH:7]=[CH:8][C:9]([CH2:10][P:11](=[O:18])([O:12][CH2:13][CH3:14])[O:15][CH2:16][CH3:17])=[CH:19][CH:20]=1)=[C:1]=[S:2]

参加物

6

反応物 4

HCID 962WaterHCID 10040ThiophosgeneHCID 88358Diethyl p-aminobenzylphosphonateHCID 516892Sodium Bicarbonate

生成物 1

HCID 22568434Diethyl 4-isothiocyanatobenzylphosphonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Thiophosgene (4.1 mL, 54 mmol) was added al at once to a mixture of diethyl 4-aminobenzylphosphonate (12.04 g, 50 mmol), sodium bicarbonate (8.33 g, 99 mmol), water (100 mL), and dichloromethane (250 mL), and the mixture was stirred at room temperature for about 2 hours. The organic and aqueous layers were separated, the organic layer dried over magnesium sulfate, filtered, and concentrated to give the product isothiocyanate as a brown oil. This was used directly in the next step.

後処理

  1. customThe organic and aqueous layers were separated
  2. dry with materialthe organic layer dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-2c8f5600ae6f41b9984d67f20d309d62
出典データセット
uspto-grants-2005_02
特許番号
US06858739B2

関連ノート

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