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Dimethylamine → HCID 11676128, 화합물

HRID 900320
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HRID 900320 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH:9][C:10]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][C:18]=3[CH2:20][N:21]3[CH2:26][CH2:25][C@@H:24]([NH:27]C(=O)OCC=C)[C@H:23]([C:34](=[O:37])[NH:35][CH3:36])[CH2:22]3)[N:13]=[CH:12][N:11]=2)[CH:6]=[CH:7][CH:8]=1.N(C)C>C1COCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[NH2:27][C@@H:24]1[CH2:25][CH2:26][N:21]([CH2:20][C:18]2[CH:17]=[CH:16][CH:15]=[C:14]3[C:19]=2[C:10]([NH:9][C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[CH:4]=2)=[N:11][CH:12]=[N:13]3)[CH2:22][C@H:23]1[C:34]([NH:35][CH3:36])=[O:37]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 674DimethylamineHCID 58711726HCID 58711726, 화합물

생성물 1

HCID 11676128HCID 11676128, 화합물

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 15E (27 mg, 0.054 mmol) in THF (3 ml) was degassed and purged with N2. To this was added 2N Me2NH in THF (95 μl, 0.19 mmol), followed by Pd(PPh3)4 (9 mg, 0.0078 mmol). The mixture was stirred at room temperature for 1.5 h. Concentration in vacuo followed by purification using preparative HPLC gave, after concentration and lyophilization, a TFA salt of 15F (20.3 mg, 70%) as a solid. The compound has an analytical HPLC retention time=1.307 min (Chromolith SpeedROD column 4.6×50 mm, 10-90% aqueous methanol containing 0.1% TFA over 4 minutes, 4 mL/min, monitoring at 254 nm) and a LC/MS M++H=421+.

후처리

  1. custompurged with N2
  2. concentrationConcentration in vacuo
  3. customfollowed by purification
  4. customgave
  5. concentrationafter concentration and lyophilization
  6. customan analytical HPLC retention time=1.307 min (Chromolith SpeedROD column 4.6×50 mm, 10-90% aqueous methanol containing 0.1% TFA over 4 minutes, 4 mL/min, monitoring at 254 nm)

출처 및 근거

ORD 기록
ord-07a4f55bc1f1474190699e3ca704c1fe
출처 데이터셋
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07358256B2

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