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Ethanol → 4-(Carboxybutyl)-4'-dodecyloxybiphenyl

HRID 36825
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HRID 36825 반응식
[CH2:1]([O:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]2[CH:25]=[CH:24][C:23]([CH2:26][CH2:27][CH2:28][CH2:29][C:30]([O:32]CC)=[O:31])=[CH:22][CH:21]=2)=[CH:16][CH:15]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].[OH-].[K+].C(O)C.O>Cl>[C:30]([CH2:29][CH2:28][CH2:27][CH2:26][C:23]1[CH:24]=[CH:25][C:20]([C:17]2[CH:18]=[CH:19][C:14]([O:13][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])=[CH:15][CH:16]=2)=[CH:21][CH:22]=1)([OH:32])=[O:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 702EthanolHCID 962WaterHCID 14797Potassium HydroxideHCID 54101004HCID 54101004, 화합물

생성물 1

HCID 542681554-(Carboxybutyl)-4'-dodecyloxybiphenyl수율 90.5%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

19 mmol of the compound from Example 15, 66.7 mmol of KOH, 100 ml of ethanol and 50 ml of water are introduced into a 500 ml single-necked flask fitted with reflux condenser and magnetic stirrer, and the mixture is refluxed for 6 hours. After cooling, the reaction mixture is carefully acidified in concentrated HCl solution and subsequently washed with water until neutral. The solvent is stripped off, and the residue is recrystallized a number of times from glacial acetic acid. The residue is then boiled with methanol and subsequently with ether and filtered off with suction. Yield: 90.5%.

후처리

  1. customfitted
  2. temperaturewith reflux condenser and magnetic stirrer
  3. temperaturethe mixture is refluxed for 6 hours
  4. temperatureAfter cooling
  5. washsubsequently washed with water until neutral
  6. customthe residue is recrystallized a number of times from glacial acetic acid
  7. filtrationfiltered off with suction

출처 및 근거

ORD 기록
ord-8e75e78528e7419c91c7087c90cc5233
출처 데이터셋
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05417884

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