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Isopropanol → 5-Phenoxy-4-methoxymethyl-beta-carboline-3-carboxylic acid isopropyl ester

HRID 2166366
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HRID 2166366 반응식
[CH2:1]([O:3][C:4]([C:6]1[N:7]=[CH:8][C:9]2[NH:10][C:11]3[C:16]([C:17]=2[C:18]=1[CH2:19][O:20][CH3:21])=[C:15]([O:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[CH:14]=[CH:13][CH:12]=3)=[O:5])[CH3:2].[CH:29](O)(C)C>[Ti+4]>[CH:1]([O:3][C:4]([C:6]1[N:7]=[CH:8][C:9]2[NH:10][C:11]3[C:16]([C:17]=2[C:18]=1[CH2:19][O:20][CH3:21])=[C:15]([O:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[CH:14]=[CH:13][CH:12]=3)=[O:5])([CH3:29])[CH3:2]
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참가 물질

4

반응물 2

HCID 3776IsopropanolHCID 138000715-Phenoxy-4-methoxymethyl-beta-carboline-3-carboxylic acid ethyl ester

생성물 1

HCID 138001015-Phenoxy-4-methoxymethyl-beta-carboline-3-carboxylic acid isopropyl ester수율 82%

시약·촉매·용매 1

HCID 114942Titanium cation (4+)촉매

실험 절차

540 mg of 5-phenoxy-4-methoxymethyl-beta-carboline-3-carboxylic acid ethyl ester in 30 ml of isopropanol is refluxed with 0.2 ml of titanium(IV) isopropylate for 2 hours. After concentration, it is mixed with 0.5N hydrochloric acid and extracted with ethyl acetate. The ethyl acetate phase is dried, filtered and concentrated and digested with diisopropyl ether. 450 mg (82% of theory) of 5-phenoxy-4-methoxymethyl-beta-carboline-3-carboxylic acid isopropyl ester with a melting point of 207°-209° C. is obtained.

후처리

  1. concentrationAfter concentration, it
  2. additionis mixed with 0.5N hydrochloric acid
  3. extractionextracted with ethyl acetate
  4. dry with materialThe ethyl acetate phase is dried
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b74cf49a576c4185baf6b4e3477a2c00
출처 데이터셋
uspto-grants-1990_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04945090

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