Dichloromethane → HCID 69199922, 화합물

HRID 132785노트

반응식

HRID 132785 반응식
[OH:1][CH:2]1[CH2:6][CH2:5][CH2:4][C:3]1([CH2:12][CH2:13][CH3:14])[C:7]([O:9][CH2:10][CH3:11])=[O:8].C(Cl)Cl.[CH3:18][C:19]1[CH:27]=[CH:26][CH:25]=[CH:24][C:20]=1[C:21](Cl)=[O:22]>N1C=CC=CC=1>[CH2:12]([C:3]1([C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:4][CH2:5][CH2:6][CH:2]1[O:1][C:21](=[O:22])[C:20]1[CH:24]=[CH:25][CH:26]=[CH:27][C:19]=1[CH3:18])[CH2:13][CH3:14]

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 702762-Methylbenzoyl chlorideHCID 69199039HCID 69199039, 화합물

생성물 1

HCID 69199922HCID 69199922, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

Ethyl 2-hydroxy-1-n-propyl-cyclopentane carboxylate (6.00 g) was diluted using 60 ml of methylene chloride. At room temperature and with magnetic stirring, pyridine (3.66 ml) was slowly added, then 2-methyl-benzoyl chloride (5.95 ml) was dropwise added. Upon the completion of the addition, the reaction was continued for 12 hours. Then solvent was removed, and the residue was extracted using ethyl acetate and water. Organic layer was washed, in turn, using 10% hydrochloric acid aqueous solution to pH of about 2, using saline solution to neutrality, using 10% aqueous solution of sodium carbonate for three times, and then using saline solution to neutrality. The organic layer was dried, and removing solvent gave 9.61 g of yellow liquid. MS: m/e 319(M+′+1), 318(M+′), 273, 259, 199, 183, 153, 119(base), 91, 77.

후처리

  1. additionUpon the completion of the addition
  2. customThen solvent was removed
  3. extractionthe residue was extracted
  4. washOrganic layer was washed, in turn
  5. customThe organic layer was dried
  6. customremoving solvent

출처 및 근거

ORD 기록
ord-95d87492fc5642e38caa99c50994e91b
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07388103B2

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