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1-Chloroethyl chloroformate → 4-[4-(4,5-Dihydro-5-phenyl-3-isoxazolyl)-2-thiazolyl]-1,2,3,6-tetrahydropyridine hydrochloride

HRID 1528556
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HRID 1528556 반응식
[C:1]1([CH:7]2[O:11][N:10]=[C:9]([C:12]3[N:13]=[C:14]([C:17]4[CH2:18][CH2:19][N:20](CC5C=CC=CC=5)[CH2:21][CH:22]=4)[S:15][CH:16]=3)[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:30]C(OC(Cl)C)=O>ClC(Cl)C>[ClH:30].[C:1]1([CH:7]2[O:11][N:10]=[C:9]([C:12]3[N:13]=[C:14]([C:17]4[CH2:18][CH2:19][NH:20][CH2:21][CH:22]=4)[S:15][CH:16]=3)[CH2:8]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
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참가 물질

4

반응물 2

HCID 5213051-Chloroethyl chloroformateHCID 687439224-[4-(4,5-Dihydro-5-phenyl-3-isoxazolyl)-2-thiazolyl]-1,2,3,6-tetrahydro-1-(phenylmethyl)pyridine2회

생성물 1

HCID 687428514-[4-(4,5-Dihydro-5-phenyl-3-isoxazolyl)-2-thiazolyl]-1,2,3,6-tetrahydropyridine hydrochloride

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

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온도
80 °C

실험 절차

To a solution of 4-[4-(4,5-dihydro-5-phenyl-3-isoxazolyl)-2-thiazolyl]-1,2,3,6-tetrahydro-1-(phenylmethyl)pyridine (i.e. the product of Example 13, Step B) (0.400 g, 0.99 mmol) in dichloroethane (10 mL) was added 1-chloroethyl chloroformate (0.286 g, 1.99 mmol), and the reaction mixture was heated to 80° C. for 5 h. The reaction mixture was cooled to room temperature and concentrated under reduced pressure. Methanol (10 mL) was added to the residue, and the resulting mixture was heated to 60° C. for 1 h, cooled to room temperature, and concentrated under reduced pressure. The residue was triturated with 50% of petroleum ether in ethyl acetate, and the solid formed was filtered and dried to give 0.25 g of the title compound as a white solid.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. concentrationconcentrated under reduced pressure
  3. additionMethanol (10 mL) was added to the residue
  4. temperaturethe resulting mixture was heated to 60° C. for 1 h
  5. temperaturecooled to room temperature
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was triturated with 50% of petroleum ether in ethyl acetate
  8. customthe solid formed
  9. filtrationwas filtered
  10. customdried

출처 및 근거

ORD 기록
ord-f04001486d7f4ba4a631675dd744c7e8
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09090604B2

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