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1,2-Dichloroethane → N-Ethylcarbamate 4,6-dichloro-5-methoxy-8-methyl-1,2,3,3a,8,8a-hexahydroindeno[1,2-c]pyrrole

HRID 508524
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HRID 508524 반응식
C1C(=O)N([Cl:8])C(=O)C1.C(O)(=O)C.[CH2:13]([NH:15][C:16](=[O:18])[O-:17])[CH3:14].[CH3:19][O:20][C:21]1C=C[C:24]2[CH:25]([CH3:33])[CH:26]3[CH2:30][NH:29][CH2:28][CH:27]3[C:31]=2[CH:32]=1.Cl[CH2:35][CH2:36][Cl:37]>>[CH2:13]([NH:15][C:16](=[O:17])[O-:18])[CH3:14].[Cl:37][C:36]1[C:35]2[CH:27]3[CH2:28][NH:29][CH2:30][CH:26]3[CH:25]([CH3:33])[C:24]=2[CH:31]=[C:32]([Cl:8])[C:21]=1[O:20][CH3:19]
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참가 물질

5

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HCID 111,2-DichloroethaneHCID 176Acetic AcidHCID 31398ChlorosuccinimideHCID 86602843N-Ethylcarbamate 5-methoxy-8-methyl-1,2,3,3a,8,8a-hexahydroindeno[1,2-c]pyrrole

생성물 1

HCID 131728821N-Ethylcarbamate 4,6-dichloro-5-methoxy-8-methyl-1,2,3,3a,8,8a-hexahydroindeno[1,2-c]pyrrole

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온도
70 °C

실험 절차

NCS (63 mg, 0.47 mmol) and acetic acid (1 mL) were added to a solution of N-ethylcarbamate-5-methoxy-8-methyl-1,2,3,3a,8,8a-hexahydroindeno[1,2-c]pyrrole (from Example 2, Step A) (43 mg, 0.16 mmol) in DCE (1 mL), and the reaction solution was stirred for 3 hours at 70° C. The reaction was quenched with H2O and the solution filtered through an Extrelut column. The column was washed with CH2Cl2, and the filtrate was concentrated. The subtitle compound was obtained without further purification. MS calculated for C16H19Cl2NO3+H: 344, observed: 344.

후처리

  1. customThe reaction was quenched with H2O
  2. filtrationthe solution filtered through an Extrelut column
  3. washThe column was washed with CH2Cl2
  4. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-2edb7e02b81242878d1f5224e547b339
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09096520B2

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