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Diethylamine → HCID 86751671, 화합물

HRID 2294897
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HRID 2294897 반응식
[CH2:1]([C:5]1[N:22]([CH2:23][C:24]2[CH:29]=[CH:28][C:27]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=3[C:36]3[N:40]([CH:41]([O:43][CH2:44][CH3:45])[CH3:42])[N:39]=[N:38][N:37]=3)=[CH:26][CH:25]=2)[C:8]2=[N:9][C:10]([C:19]([OH:21])=[O:20])=[C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=3)[CH:12]=[C:7]2[N:6]=1)[CH2:2][CH2:3][CH3:4].C(NCC)C>C(Cl)Cl.CN(C1C=CN=CC=1)C>[CH2:5]([N-:6][CH2:7][CH3:12])[CH3:1].[CH2:1]([C:5]1[N:22]([CH2:23][C:24]2[CH:29]=[CH:28][C:27]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=3[C:36]3[N:40]([CH:41]([O:43][CH2:44][CH3:45])[CH3:42])[N:39]=[N:38][N:37]=3)=[CH:26][CH:25]=2)[C:8]2=[N:9][C:10]([C:19]([O-:21])=[O:20])=[C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=3)[CH:12]=[C:7]2[N:6]=1)[CH2:2][CH2:3][CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 8021DiethylamineHCID 21472368HCID 21472368, 화합물

생성물 1

HCID 86751671HCID 86751671, 화합물수율 77.6%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

80 mg (0.13 mmole) of the compound obtained in step 1 was dissolved in 2 ml of CH2Cl2 and to the resulting solution were added 12 mg (0.16 mmole) of diethylamine, 33 mg (0.16 mmole) of DDC(Dithiocarb Sodium) and 2 mg (0.016 mmole) of DMAP. The resultant was stirred for 16 hours at room temperature and evaporated under reduced pressure to remove the residual solvent. The residue was purified with column chromatography (ethyl acetate) to obtain 34 mg of the title compound (yield 40%).

후처리

  1. customevaporated under reduced pressure
  2. customto remove the residual solvent
  3. customThe residue was purified with column chromatography (ethyl acetate)

출처 및 근거

ORD 기록
ord-d31bc1b910704efdaaf6d668109c6fa1
출처 데이터셋
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05691348

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