Water → HCID 86584489、化合物

HRID 394941ノート

反応式

HRID 394941 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])[C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:4][CH:3]=1.[CH3:19][C:20]([CH3:25])=[CH:21][C:22](Cl)=[O:23].O>C(Cl)(Cl)Cl>[CH3:19][C:20]([CH3:25])=[CH:21][C:22]([NH:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]([CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])[C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:6][CH:7]=1)=[O:23]

参加物

5

反応物 3

HCID 962WaterHCID 1023943-Methyl-2-butenoyl chlorideHCID 86584488(RS)-ethyl 2-(4-aminophenyl)-heptanoate

生成物 1

HCID 86584489HCID 86584489、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

10.4 g of (RS)-ethyl 2-(4-aminophenyl)-heptanoate dissolved in 100 ml of chloroform was treated dropwise with 4.64 ml of 3,3-dimethylacryloyl chloride. The mixture was heated to reflux for 6 hours. After cooling to room temperature, 100 ml of water were added. The phases were separated and the aqueous phase was extracted with two portions of 50 ml of chloroform. The combined organic extracts were washed with two portions of 100 ml of saturated aqueous sodium bicarbonate solution and one portion of 100 ml of saturated aqueous sodium chloride solution. The organic phase was dried over MgSO4 and concentrated in vacuo. The product was used without purification. 1H NMR (CDCl3): 7.48 (br. d, J=8.4 Hz, 2H), 7.39 (br. s, 1H), 7.24 (d, J=8.5 Hz, 2H), 5.71 (br. s, 1H), 4.20-4.00 (m, 2H), 3.48 (t, J=7.7 Hz, 1H), 2.21 (br. s, 3H), 2.15-1.95 (m, 1H), 1.87 (s, 3H), 1.80-1.65 (m, 1H), 1.35-1.15 (m, 6H), 1.20 (t, J=7.1 Hz, 3H), 0.85 (t, J=6.7 Hz, 3H).

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 6 hours
  3. customThe phases were separated
  4. extractionthe aqueous phase was extracted with two portions of 50 ml of chloroform
  5. washThe combined organic extracts were washed with two portions of 100 ml of saturated aqueous sodium bicarbonate solution and one portion of 100 ml of saturated aqueous sodium chloride solution
  6. dry with materialThe organic phase was dried over MgSO4
  7. concentrationconcentrated in vacuo
  8. customThe product was used without purification

出典と根拠

ORDレコード
ord-d46f49955f834abdb392f90bcef21165
出典データセット
uspto-grants-2003_08
特許番号
US06603012B2

反応ノート

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