Dichloromethane → HCID 69199302、化合物

HRID 132784ノート

反応式

HRID 132784 の反応式
[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.[C:18](Cl)(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>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:18](=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:13][CH3:14]

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 7412Benzoyl chlorideHCID 69199039HCID 69199039、化合物

生成物 1

HCID 69199302HCID 69199302、化合物収率 109.7%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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 (3.67 ml) was slowly added, then benzoyl chloride (5.33 ml, 0.045 mol) 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 10.00 g of yellow liquid, MS: m/e 305(M+″+1), 304(M+), 259, 230, 199, 182, 153, 105(base), 77.

後処理

  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

出典と根拠

ORDレコード
ord-90e94606c10848aa9461dfd9716f389c
出典データセット
uspto-grants-2008_06
特許番号
US07388103B2

反応ノート

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