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

HRID 563049

반응식

HRID 563049 반응식
[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]

참가 물질

5

반응물 3

HCID 949N,N-DimethylanilineHCID 4943PropofolHCID 6371Phosgene

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d02b3c3fdfdd4b3691ca89641b90487c
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08067455B2

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