HCID 59568585, 화합물 → HCID 49783984, 화합물

HRID 216972노트

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HRID 216972 반응식
[C:1]([C@@H:3]([NH:27][C:28]([C:30]1([NH:36]C(=O)OC(C)(C)C)[CH2:35][CH2:34][O:33][CH2:32][CH2:31]1)=[O:29])[CH2:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[CH:15][C:14]([S:17]([N:20]3[CH2:25][CH2:24][N:23]([CH3:26])[CH2:22][CH2:21]3)(=[O:19])=[O:18])=[CH:13][CH:12]=2)=[CH:7][CH:6]=1)#[N:2]>C(O)=O>[NH2:36][C:30]1([C:28]([NH:27][C@H:3]([C:1]#[N:2])[CH2:4][C:5]2[CH:6]=[CH:7][C:8]([C:11]3[CH:12]=[CH:13][C:14]([S:17]([N:20]4[CH2:21][CH2:22][N:23]([CH3:26])[CH2:24][CH2:25]4)(=[O:18])=[O:19])=[CH:15][CH:16]=3)=[CH:9][CH:10]=2)=[O:29])[CH2:35][CH2:34][O:33][CH2:32][CH2:31]1

참가 물질

3

반응물 1

HCID 59568585HCID 59568585, 화합물

생성물 1

HCID 49783984HCID 49783984, 화합물수율 20.6%

시약·촉매·용매 1

HCID 284Formic Acid용매

실험 절차

(S)-tert-Butyl 4-(1-cyano-2-(4′-(4-methylpiperazin-1-ylsulfonyl)biphenyl-4-yl)ethylcarbamoyl)tetrahydro-2H-pyran-4-ylcarbamate (Example 29, step (ii), 250 mg) in formic acid (2 mL) was heated at 50° C. for 20 min. Volatiles were removed under reduced pressure and then azeotroped with methanol. The product was purified by reversed phase HPLC using methanol in 0.1% aqueous TFA as eluent. The residue was converted to the free base by elution through a PL-HCO3 MP cartridge in dichloromethane/methanol to afford the titled compound (43 mg).

후처리

  1. customVolatiles were removed under reduced pressure
  2. customazeotroped with methanol
  3. customThe product was purified by reversed phase
  4. washThe residue was converted to the free base by elution through a PL-HCO3 MP cartridge in dichloromethane/methanol

출처 및 근거

ORD 기록
ord-2958ae81ec7340fa9ac4497958f20ba2
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08193239B2

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