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Diethylamine → 1636-15-3

HRID 748598
ノート
印刷プレビュー

反応式

HRID 748598 の反応式
[C:1]1([P:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)Cl)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:15]([NH:17][CH2:18][CH3:19])[CH3:16]>C1(C)C=CC=CC=1>[P:7]([N:17]([CH2:18][CH3:19])[CH2:15][CH3:16])([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 8021DiethylamineHCID 66180Chlorodiphenylphosphine

生成物 1

HCID 121407181636-15-3

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Diphenylchlorophosphine (2.0 mL, 2.38 g, 10.79 mmol) was added to a stirred solution of diethylamine (2.5 mL, 1.82 g, 24.9 mmol) in toluene (20 mL). The resulting white slurry was stirred overnight at ambient temperature and filtered. The filtered solid was washed with toluene (2×10 mL). The combined filtrate was reduced in volume by distillation in vacuum to approximately 20 mL and transferred to a graduated Schlenk tube equipped with a Yong valve. The volume of the solution was adjusted to 31.0 mL by addition of toluene to give 0.348 M solution of Ph2PNEt2. 31P{1H} NMR (toluene, 25° C.), δ: 51.0 (s).

後処理

  1. filtrationfiltered
  2. washThe filtered solid was washed with toluene (2×10 mL)
  3. distillationThe combined filtrate was reduced in volume by distillation in vacuum to approximately 20 mL
  4. customtransferred to a graduated Schlenk tube
  5. customequipped with a Yong valve
  6. additionThe volume of the solution was adjusted to 31.0 mL by addition of toluene

出典と根拠

ORDレコード
ord-a36931dd06a24e8c920955b10b7087e3
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07399859B1

反応ノート

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