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Potassium Hydroxide → HCID 117667602, 화합물

HRID 712586
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HRID 712586 반응식
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[N:10][CH:11]=1)[NH:8][CH2:7][CH2:6][CH2:5]2.ClC(Cl)(Cl)[C:14]([N:16]=C=O)=[O:15].[OH-].[K+]>C(Cl)Cl>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[N:10][CH:11]=1)[N:8]([C:14]([NH2:16])=[O:15])[CH2:7][CH2:6][CH2:5]2
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참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 76400Trichloroacetyl isocyanateHCID 179301266-Bromo-1,2,3,4-tetrahydro-1,8-naphthyridine

생성물 1

HCID 117667602HCID 117667602, 화합물수율 96.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

To a cooled (0° C.) solution of 6-bromo-1,2,3,4-tetrahydro-[1,8]naphthyridine (6.4 g, 30.0 mmol) in DCM (75 mL) is added a trichloroacetyl isocyanate (3.8 mL, 31.5 mmol). After stirring for 1 h at 0° C., a solution of methanolic KOH (1M, 10 mL) is added. The resulting mixture is allowed to warm and stir at room temperature for 16 h. The reaction is concentrated and purified by silica gel column (0-100% EtOAc in heptane) to afford the title compound (7.4 g).

후처리

  1. temperatureto warm
  2. stirringstir at room temperature for 16 h
  3. concentrationThe reaction is concentrated
  4. custompurified by silica gel column (0-100% EtOAc in heptane)

출처 및 근거

ORD 기록
ord-10fb7eb43d054d6da54d6dc2c3f65a8e
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181272B2

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