Hydrochloric Acid → HCID 178485823、化合物

HRID 333497

反応式

HRID 333497 の反応式
[Cl:1]CCl.CO.[CH3:6][O:7][C:8](=[O:64])[NH:9][C@H:10]([C:14]([N:16]1[CH2:20][CH2:19][CH2:18][C@H:17]1[C:21]1[NH:22][CH:23]=[C:24]([C:26]2[CH:31]=[CH:30][C:29]([C:32]3[CH:37]=[CH:36][C:35]([NH:38][C:39]([C:41]4[CH:42]=[N:43][C:44]([N:47]5[CH2:52][C@H:51]([CH3:53])[N:50]([C:54](=[O:57])[NH:55][CH3:56])[CH2:49][C@H:48]5[CH3:58])=[CH:45][CH:46]=4)=[O:40])=[CH:34][C:33]=3[O:59][C:60]([F:63])([F:62])[F:61])=[CH:28][CH:27]=2)[N:25]=1)=[O:15])[CH:11]([CH3:13])[CH3:12].[ClH:65]>COC1CCCC1>[ClH:1].[ClH:65].[CH3:6][O:7][C:8](=[O:64])[NH:9][C@H:10]([C:14]([N:16]1[CH2:20][CH2:19][CH2:18][C@H:17]1[C:21]1[NH:22][CH:23]=[C:24]([C:26]2[CH:27]=[CH:28][C:29]([C:32]3[CH:37]=[CH:36][C:35]([NH:38][C:39]([C:41]4[CH:42]=[N:43][C:44]([N:47]5[CH2:52][C@H:51]([CH3:53])[N:50]([C:54](=[O:57])[NH:55][CH3:56])[CH2:49][C@H:48]5[CH3:58])=[CH:45][CH:46]=4)=[O:40])=[CH:34][C:33]=3[O:59][C:60]([F:63])([F:61])[F:62])=[CH:30][CH:31]=2)[N:25]=1)=[O:15])[CH:11]([CH3:12])[CH3:13]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 6344DichloromethaneHCID 178485822HCID 178485822、化合物

生成物 1

HCID 178485823HCID 178485823、化合物

試薬・触媒・溶媒 1

HCID 138539Cyclopentyl methyl ether溶媒

反応条件

温度
3 °C

実験手順

Dichloromethane (100 mL) and methanol (50 mL) were added to ((S)-1-{(S)-2-[4-(4′-{[6-((2R,5S)-2,5-dimethyl-4-methylcarbamoyl-piperazin-1-yl)-pyridine-3-carbonyl]-amino}-2′-trifluoromethoxy-biphenyl-4-yl)-1H-imidazol-2-yl]-pyrrolidine-1-carbonyl}-2-methyl-propyl)-carbamic acid methyl ester (10.17 g, 12.40 mmol) and the solution was stirred for 10 min, then cooled to 3° C. and 3 M of HCl in cyclopentyl methyl ether (12.4 mL) was added dropwise keeping the temperature of the reaction mixture less than 10° C. The water bath was removed and the reaction mixture was stirred for 15 min, and concentrated to about 50 mL. Isopropyl acetate was added and the mixture was concentrated to dryness. The resulting material was vacuum dried at RT overnight and vacuum oven dried at RT over the weekend to provide the title compound (12.2 g).

後処理

  1. customthe temperature of the reaction mixture less than 10° C
  2. customThe water bath was removed
  3. stirringthe reaction mixture was stirred for 15 min
  4. concentrationconcentrated to about 50 mL
  5. additionIsopropyl acetate was added
  6. concentrationthe mixture was concentrated to dryness
  7. customdried at RT overnight
  8. customvacuum oven dried at RT over the weekend

出典と根拠

ORDレコード
ord-939c810fe3974aa9a487298711c8c219
出典データセット
uspto-grants-2014_11
特許番号
US08883135B2

関連ノート

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