Methyl N-(triethylammoniosulfonyl)carbamate → HCID 59568585, 화합물

HRID 216971노트

반응식

HRID 216971 반응식
[NH2:1][C:2](=O)[C@@H:3]([NH:27][C:28]([C:30]1([NH:36][C:37](=[O:43])[O:38][C:39]([CH3:42])([CH3:41])[CH3:40])[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.CC[N+](S(N=C(OC)[O-])(=O)=O)(CC)CC>ClCCl>[C:2]([C@@H:3]([NH:27][C:28]([C:30]1([NH:36][C:37](=[O:43])[O:38][C:39]([CH3:41])([CH3:40])[CH3:42])[CH2:35][CH2:34][O:33][CH2:32][CH2:31]1)=[O:29])[CH2:4][C:5]1[CH:6]=[CH:7][C:8]([C:11]2[CH:12]=[CH:13][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:15][CH:16]=2)=[CH:9][CH:10]=1)#[N:1]

참가 물질

4

반응물 2

HCID 2724994Methyl N-(triethylammoniosulfonyl)carbamateHCID 59568627HCID 59568627, 화합물

생성물 1

HCID 59568585HCID 59568585, 화합물수율 96.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

(S)-tert-Butyl 4-(1-amino-3-(4′-(4-methylpiperazin-1-ylsulfonyl)biphenyl-4-yl)-1-oxopropan-2-ylcarbamoyl)tetrahydro-2H-pyran-4-ylcarbamate (Example 29, step (i), 267 mg) in dichloromethane (10 mL) was treated with Burgess' reagent (202 mg) and the mixture was stirred at room temperature for 18 h. The solvent was partially evaporated under reduced pressure and the mixture was purified by chromatography on silica eluting with methanol/dichloromethane (0:100 to 5:95), triethylamine/methanol/dichloromethane (1:5:95) to afford the sub-titled compound (250 mg).

후처리

  1. customThe solvent was partially evaporated under reduced pressure
  2. customthe mixture was purified by chromatography on silica eluting with methanol/dichloromethane (0:100 to 5:95), triethylamine/methanol/dichloromethane (1:5:95)

출처 및 근거

ORD 기록
ord-e39a55fa601d45c3bd23985a540f824e
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08193239B2

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