Methyl N-(triethylammoniosulfonyl)carbamate → HCID 59568585、化合物

HRID 216971ノート

反応式

HRID 216971 の反応式
[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]

参加物

4

反応物 2

HCID 2724994Methyl N-(triethylammoniosulfonyl)carbamateHCID 59568627HCID 59568627、化合物

生成物 1

HCID 59568585HCID 59568585、化合物収率 96.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

(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).

後処理

  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)

出典と根拠

ORDレコード
ord-e39a55fa601d45c3bd23985a540f824e
出典データセット
uspto-grants-2012_06
特許番号
US08193239B2

反応ノート

読み込み中…