Phenothiazine → 1-Methylheptyl acrylate

HRID 131777

반응식

HRID 131777 반응식
[CH3:1][CH:2]([OH:9])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[OH2:10].[C:11]1([CH3:21])C=CC(S(O)(=O)=O)=C[CH:12]=1.C1C2NC3C(=CC=CC=3)SC=2C=CC=1>C1(C)C=CC=CC=1>[C:21]([O:9][CH:2]([CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8])[CH3:1])(=[O:10])[CH:11]=[CH2:12]

참가 물질

5

반응물 3

HCID 7108PhenothiazineHCID 200832-OctanolHCID 521998p-Toluenesulfonic acid monohydrate

생성물 1

HCID 980551-Methylheptyl acrylate

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 2-octanol (268.51 grams, 2.1 mol), AA (183.75 grams, 2.6 mol), p-toluenesulfonic acid monohydrate (5.00 grams, 26 mmol), toluene (250 grams) and phenothiazine (1.0 grams) was heated to reflux. Water was separated from the toluene/water azeotrope using a Dean Stark distillation trap. After six hours at reflux a total of 37 milliliters of water was collected in the trap. The reaction mixture was washed with 1 Molar aqueous sodium hydroxide (200 milliliters), then concentrated under reduced pressure. The remaining oil was distilled under reduced pressure (65-67° C. at 2 mmHg) to give the product as a colorless oil. (Yield: 248.6 grams)

후처리

  1. temperaturewas heated to reflux
  2. customWater was separated from the toluene/water
  3. distillationa Dean Stark distillation trap
  4. temperatureAfter six hours at reflux a total of 37 milliliters of water
  5. customwas collected in the trap
  6. washThe reaction mixture was washed with 1 Molar aqueous sodium hydroxide (200 milliliters)
  7. concentrationconcentrated under reduced pressure
  8. distillationThe remaining oil was distilled under reduced pressure (65-67° C. at 2 mmHg)

출처 및 근거

ORD 기록
ord-db3240e846d947fe850b42518ed511a3
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07385020B2

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