Ethylamine → HCID 53233982, 화합물

HRID 1942219

반응식

HRID 1942219 반응식
[CH:1]1([C:4]2[CH:9]=[CH:8][C:7]([N:10]3[CH2:14][CH2:13][C:12]4([CH2:19][CH2:18][N:17]([CH2:20][C:21](O)=[O:22])[CH2:16][CH2:15]4)[C:11]3=[O:24])=[CH:6][CH:5]=2)[CH2:3][CH2:2]1.CN(C(O[N:33]1N=N[C:35]2C=CC=C[C:34]1=2)=[N+](C)C)C.[B-](F)(F)(F)F.CCN(CC)CC.C(N)C>CN(C=O)C>[CH:1]1([C:4]2[CH:5]=[CH:6][C:7]([N:10]3[CH2:14][CH2:13][C:12]4([CH2:15][CH2:16][N:17]([CH2:20][C:21]([NH:33][CH2:34][CH3:35])=[O:22])[CH2:18][CH2:19]4)[C:11]3=[O:24])=[CH:8][CH:9]=2)[CH2:2][CH2:3]1

참가 물질

6

반응물 4

HCID 6341EthylamineHCID 8471TriethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 58287265[2-(4-Cyclopropyl-phenyl)-1-oxo-2,8-diaza-spiro[4.5]dec-8-yl]-acetic acid

생성물 1

HCID 53233982HCID 53233982, 화합물수율 35.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of mg 42.7 mg (0.13 mmol) [2-(4-Cyclopropyl-phenyl)-1-oxo-2,8-diaza-spiro[4.5]dec-8-yl]-acetic acid, 54.2 mg (0.195 mmol) TBTU, 26 mg (0.26 mmol) NEt3 and 8.7 mg (0.195 mmol) ethylamine in 2 mL DMF was stirred at room temperature for 16 h and evaporated to dryness. The residue was taken up in DMF and subjected to purification by preparative HPLC on reversed phase eluting with a gradient formed from acetonitrile, water and NEt3. The product containing fractions were evaporated to yield 16.2 mg (35%) of the title compound. MS m/e: 356.3 [M+H]+.

후처리

  1. customevaporated to dryness
  2. customsubjected to purification by preparative HPLC on reversed phase
  3. washeluting with a gradient
  4. customformed from acetonitrile, water and NEt3
  5. additionThe product containing fractions
  6. customwere evaporated

출처 및 근거

ORD 기록
ord-34df0b0f187547429eb0857cdc1aab71
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08389539B2

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