N,N-Dimethylaniline → 2,6-Di(propan-2-yl)phenyl carbonochloridate

HRID 563049

反応式

HRID 563049 の反応式
[CH3:1][CH:2]([C:4]1[CH:5]=[CH:6][CH:7]=[C:8]([CH:11]([CH3:13])[CH3:12])[C:9]=1[OH:10])[CH3:3].[C:14](Cl)([Cl:16])=[O:15].CN(C)C1C=CC=CC=1>C1(C)C=CC=CC=1>[CH:11]([C:8]1[CH:7]=[CH:6][CH:5]=[C:4]([CH:2]([CH3:1])[CH3:3])[C:9]=1[O:10][C:14]([Cl:16])=[O:15])([CH3:13])[CH3:12]

参加物

5

反応物 3

HCID 949N,N-DimethylanilineHCID 4943PropofolHCID 6371Phosgene

生成物 1

HCID 2716192,6-Di(propan-2-yl)phenyl carbonochloridate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a cooled (0° C.) solution of propofol (20.0 g, 112 mmol) in toluene (40 mL) was added phosgene (82 mL, 20% in toluene) under a nitrogen atmosphere. The reaction mixture was stirred for 5 min, and then N,N-dimethylaniline (15 mL, 118 mmol) was added dropwise. The mixture was allowed to warm to room temperature slowly and stirred for 14 h. The suspended mixture was then filtered. The filtrate was collected and the solvent was removed in vacuo. The remaining crude product (9) was carried to the next step without further purification. 1H-NMR (400 MHz, CDCl3): δ 7.18-7.29 (m, 3H), 3.00-3.07 (m, 2H), 1.25-1.27 (d, J=6.8 Hz, 12H).

後処理

  1. stirringstirred for 14 h
  2. filtrationThe suspended mixture was then filtered
  3. customThe filtrate was collected
  4. customthe solvent was removed in vacuo
  5. customThe remaining crude product (9) was carried to the next step without further purification

出典と根拠

ORDレコード
ord-d02b3c3fdfdd4b3691ca89641b90487c
出典データセット
uspto-grants-2011_11
特許番号
US08067455B2

関連ノート

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