Dichloromethane → HCID 131716472, 화합물

HRID 2166002

반응식

HRID 2166002 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])C(Cl)=O.[OH:24][C:25]1[CH:30]=[CH:29][C:28](C2C=CC(C(OC[C@@H](C)CC)=O)=CC=2)=[CH:27][CH:26]=1.C(Cl)Cl.[C:48](OCC)(=[O:50])C>N1C=CC=CC=1>[F:1][C:2]1[C:10]([O:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])=[C:9]([CH:8]=[CH:4][CH:3]=1)[C:48]([O:24][C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1)=[O:50]

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 8857Ethyl AcetateHCID 139075384'-[(S)-2-methylbutoxycarbonyl]biphenyl-4-olHCID 150952233-Fluoro-4-dodecyloxybenzoic acid chloride

생성물 1

HCID 131716472HCID 131716472, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

3-Fluoro-4-dodecyloxybenzoic acid chloride (3.32 g: 10 mmols) and 2.84 g (10 mmols) of (S)-2-methylbutyl 4'-hydroxybiphenyl-4-carboxylate were reacted in 10 ml of pyridine and 15 ml of methylene chloride for 3 hours under reflux. After the reaction mixture was left to cool, 50 ml of ethyl acetate was added, and washed twice with 10% hydrochloric acid and once with each of a saturated sodium bicarbonate aqueous solution, water and a saturated sodium chloride aqueous solution. After the reaction product was dried with anhydrous sodium sulfate, the solvent was concentrated. Crude crystals obtained were purified by silica gel column chromatography (solvent: chloroform-hexane), and recrystallized from ethanol to obtain 4.64 g of 4{(S)-2-methylbutyloxycarbonyl]phenyl)phenyl 3-fluoro-dodecyloxybenzoate.

후처리

  1. waitAfter the reaction mixture was left
  2. temperatureto cool
  3. washwashed twice with 10% hydrochloric acid
  4. dry with materialAfter the reaction product was dried with anhydrous sodium sulfate
  5. concentrationthe solvent was concentrated
  6. customCrude crystals obtained
  7. customwere purified by silica gel column chromatography (solvent: chloroform-hexane)
  8. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-8fd63501fdbe4a128189ddda3b992b1f
출처 데이터셋
uspto-grants-1990_07
특허 번호
US04943386

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