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Tributylamine → HCID 86760712, 화합물

HRID 747759
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HRID 747759 반응식
[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][CH:14]([O:17][C:18]2[CH:23]=[CH:22][C:21]([CH2:24][C@H:25]([NH:36][S:37]([C:40]3[CH:45]=[CH:44][C:43](I)=[CH:42][CH:41]=3)(=[O:39])=[O:38])[CH2:26][O:27][C:28]3[CH:29]=[C:30]([CH:33]=[CH:34][CH:35]=3)[C:31]#[N:32])=[CH:20][CH:19]=2)[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:47]([O:51][CH2:52][CH3:53])(=[O:50])[CH:48]=[CH2:49].C1(C)C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.C(N(CCCC)CCCC)CCC>C(#N)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.ClCCl>[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][CH:14]([O:17][C:18]2[CH:23]=[CH:22][C:21]([CH2:24][C@H:25]([NH:36][S:37]([C:40]3[CH:45]=[CH:44][C:43](/[CH:49]=[CH:48]/[C:47]([O:51][CH2:52][CH3:53])=[O:50])=[CH:42][CH:41]=3)(=[O:39])=[O:38])[CH2:26][O:27][C:28]3[CH:35]=[CH:34][CH:33]=[C:30]([C:31]#[N:32])[CH:29]=3)=[CH:20][CH:19]=2)[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 7622TributylamineHCID 8821Ethyl AcrylateHCID 80271Tri-o-tolylphosphineHCID 68830378HCID 68830378, 화합물

생성물 1

HCID 86760712HCID 86760712, 화합물

시약·촉매·용매 3

HCID 167845palladium(II) acetate촉매
HCID 6342
Acetonitrile
용매
HCID 6344Dichloromethane용매

실험 절차

738 mg (1.00 mmol)) of 3-[(2S)-3-[4-[1-(benzyloxycarbonyl)-4-piperidyloxy]phenyl]-2-(4-iodobenzenesulfonylamino)propoxy]benzonitrile was dissolved in 5 ml of acetonitrile. 0.22 ml (2.0 mmol) of ethyl acrylate, 11 mg (0.05 mmol) of palladium acetate, 91 mg (0.3 mmol) of tris-o-tolylphosphine and 0.48 ml (2.0 mmol) of tributylamine were added to the solution, and they were heated under reflux for 15 hours. After the same isolation process as that of step 1 in Example 1 with dichloromethane as the extractant, the crude product was obtained, which was purified by the silica gel column chromatography to obtain the title compound.

후처리

  1. temperaturewere heated
  2. temperatureunder reflux for 15 hours
  3. customwhich was purified by the silica gel column chromatography

출처 및 근거

ORD 기록
ord-a99ecdb2533a474dade974fc8788f1d9
출처 데이터셋
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07396844B1

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