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Water → 3-Carbamoylisoxazol-5-ylmethyl (-)-(R)-3-(naphth-2-yloxymethyl)pyrrolidine-1-carboxylate

HRID 1466003
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HRID 1466003 반응식
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[O:11][CH2:12][C@@H:13]1[CH2:17][CH2:16][NH:15][CH2:14]1.[C:18](=O)([O:29]C1C=CC([N+]([O-])=O)=CC=1)[O:19][CH2:20][C:21]1[O:25][N:24]=[C:23]([C:26](=[O:28])[NH2:27])[CH:22]=1.CN1CCOCC1.O>ClCCl>[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[O:11][CH2:12][C@@H:13]1[CH2:17][CH2:16][N:15]([C:18]([O:19][CH2:20][C:21]2[O:25][N:24]=[C:23]([C:26](=[O:28])[NH2:27])[CH:22]=2)=[O:29])[CH2:14]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 79724-MethylmorpholineHCID 26192527(R)-3-(naphth-2-yloxymethyl)pyrrolidineHCID 666608603-Carbamoylisoxazol-5-ylmethyl 4-nitrophenyl carbonate

생성물 1

HCID 673509143-Carbamoylisoxazol-5-ylmethyl (-)-(R)-3-(naphth-2-yloxymethyl)pyrrolidine-1-carboxylate수율 38.5%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

0.21 g (0.92 mmol) of (R)-3-(naphth-2-yloxymethyl)-pyrrolidine is dissolved in 3.80 ml of dichloromethane and then 0.31 g (1.01 mmol) of 3-carbamoylisoxazol-5-ylmethyl 4-nitrophenyl carbonate and 0.15 ml (1.38 mmol) of N-methylmorpholine are added. The mixture is stirred at ambient temperature for 20 hours and then water is added to the reaction medium. After extraction of the aqueous phase with dichloromethane, the organic phases are successively washed three times with a 1M aqueous sodium hydroxide solution and then twice with a saturated aqueous ammonium chloride solution. After having dried the organic phases over sodium sulphate, they are filtered and the filtrate is evaporated to dryness. 0.14 g of the desired product is thus obtained in the form of a white solid after purification on a column of silica gel, elution being carried out with a dichloromethane/methanol mixture, and then taken up in isopropyl ether.

후처리

  1. extractionAfter extraction of the aqueous phase with dichloromethane
  2. washthe organic phases are successively washed three times with a 1M aqueous sodium hydroxide solution
  3. dry with materialAfter having dried the organic phases over sodium sulphate, they
  4. filtrationare filtered
  5. customthe filtrate is evaporated to dryness

출처 및 근거

ORD 기록
ord-a9c4d1cdfe134fa2be194f04004afc87
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09000010B2

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