Triethylamine → tert-Butyl 2-[4-(3,4-dichlorophenoxy)-1-piperidinyl]ethylcarbamate

HRID 915544노트

반응식

HRID 915544 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]=[CH:13][C:14]=1[Cl:15])[O:5][CH:6]1[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1.C(N(CC)CC)C.Br[CH2:24][CH2:25][NH:26][C:27](=[O:33])[O:28][C:29]([CH3:32])([CH3:31])[CH3:30].C(OCC)C.O>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]=[CH:13][C:14]=1[Cl:15])[O:5][CH:6]1[CH2:11][CH2:10][N:9]([CH2:24][CH2:25][NH:26][C:27](=[O:33])[O:28][C:29]([CH3:32])([CH3:31])[CH3:30])[CH2:8][CH2:7]1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 37320424-(3,4-Dichlorophenoxy)piperidineHCID 4103526tert-Butyl N-(2-bromoethyl)carbamateHCID 21584184Diethylether water

생성물 1

HCID 22322299tert-Butyl 2-[4-(3,4-dichlorophenoxy)-1-piperidinyl]ethylcarbamate수율 73.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4-(3,4-Dichlorophenoxy)piperidine (8.6 g) was dissolved in DMF (60 ml) and triethylamine (12 ml) was added. 1,1-Dimethylethyl (2-bromoethyl)-carbamate (7.8 g) was added and the solution was stirred at room temperature for 12 hours. Diethyl ether/water (1:1500 ml) was added and the organic phase was separated, dried (MgSO4) and evaporated. Purification by chromatography (dichloromethane: methanol: NH3 (aq) 98.5:1:0.5) gave the subtitle compound (10 g).

후처리

  1. customthe organic phase was separated
  2. dry with materialdried (MgSO4)
  3. customevaporated
  4. customPurification by chromatography (dichloromethane: methanol: NH3 (aq) 98.5:1:0.5)

출처 및 근거

ORD 기록
ord-dfafd855cb834ede8fd96a2c53afdccb
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07265227B2

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