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Potassium Iodide → (3R,4R)-3-[1-(2-acetylamino-ethyl)-1,2,3,4-tetrahydro-quinolin-7-ylmethoxy]-4-[4-[3-(2-methoxy-benzyloxy)-propoxy]-phenyl]-piperidine-1-carboxylic acid tert-butyl ester

HRID 1531480
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HRID 1531480 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][C@H:11]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH2:21][CH2:22][CH2:23][O:24][CH2:25][C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=3[O:32][CH3:33])=[CH:16][CH:15]=2)[C@@H:10]([O:34][CH2:35][C:36]2[CH:45]=[C:44]3[C:39]([CH2:40][CH2:41][CH2:42][NH:43]3)=[CH:38][CH:37]=2)[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl[CH2:47][CH2:48][NH:49][C:50](=[O:52])[CH3:51].C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+]>C(#N)C>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][C@H:11]([C:14]2[CH:15]=[CH:16][C:17]([O:20][CH2:21][CH2:22][CH2:23][O:24][CH2:25][C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=3[O:32][CH3:33])=[CH:18][CH:19]=2)[C@@H:10]([O:34][CH2:35][C:36]2[CH:45]=[C:44]3[C:39]([CH2:40][CH2:41][CH2:42][N:43]3[CH2:47][CH2:48][NH:49][C:50](=[O:52])[CH3:51])=[CH:38][CH:37]=2)[CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
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참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 81815N-(2-Chloroethyl)acetamideHCID 57314360(3R,4R)-4-[4-[3-(2-methoxy-benzyloxy)-propoxy]-phenyl]-3-(1,2,3,4-tetrahydro-quinolin-7-ylmethoxy)-piperidine-1-carboxylic acid tert-butylester

생성물 1

HCID 11262561
(3R,4R)-3-[1-(2-acetylamino-ethyl)-1,2,3,4-tetrahydro-quinolin-7-ylmethoxy]-4-[4-[3-(2-methoxy-benzyloxy)-propoxy]-phenyl]-piperidine-1-carboxylic acid tert-butyl ester
수율 39.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of 2.07 g (3.36 mmol) of (3R,4R)-4-[4-[3-(2-methoxy-benzyloxy)-propoxy]-phenyl]-3-(1,2,3,4-tetrahydro-quinolin-7-ylmethoxy)-piperidine-1-carboxylic acid tert-butyl ester in 6 ml of acetonitrile was treated successively with 0.82 g (6.72 mmol, 2.0 equiv.) of N-2-chloroethyl acetamide, 0.53 g (5.04 mmol, 1.5 equiv.) of anhydrous sodium carbonate, and 0.056 g (0.34 mmol, 0.1 equiv.) of potassium iodide. This mixture was refluxed for 48 hours. Subsequently, it was poured into 100 ml of an ice/water mixture and extracted three times with 50 ml of ethyl acetate. The combined organic phases were washed three times with 20 ml of water, dried over magnesium sulphate, evaporated under reduced pressure and dried in a high vacuum. The thus-obtained crude product was separated on silica gel using ethyl acetate as the eluent and yielded 0.91 g (1.30 mmol, 39.2% of theory) of (3R,4R)-3-[1-(2-acetylamino-ethyl)-1,2,3,4-tetrahydro-quinolin-7-ylmethoxy]-4-[4-[3-(2-methoxy-benzyloxy)-propoxy]-phenyl]-piperidine-1-carboxylic acid tert-butyl ester as a yellow oil; MS: 702 (M+H)+.

후처리

  1. temperatureThis mixture was refluxed for 48 hours
  2. extractionextracted three times with 50 ml of ethyl acetate
  3. washThe combined organic phases were washed three times with 20 ml of water
  4. dry with materialdried over magnesium sulphate
  5. customevaporated under reduced pressure
  6. customdried in a high vacuum
  7. customThe thus-obtained crude product
  8. customwas separated on silica gel

출처 및 근거

ORD 기록
ord-139733c072824a0791028954d1a631fc
출처 데이터셋
uspto-grants-2001_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06197959B1

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