Hydrochloric Acid → HCID 69545788、化合物

HRID 2086297ノート

反応式

HRID 2086297 の反応式
C(OC([NH:8][C@H:9]1[CH2:13][CH2:12][N:11]([NH:14][CH:15]2[CH2:20][CH2:19][N:18]([C:21]3[CH:26]=[CH:25][N:24]=[CH:23][CH:22]=3)[CH2:17][CH2:16]2)[C:10]1=[O:27])=O)(C)(C)C.Cl.[CH3:29][O:30][C:31]1[CH:40]=[C:39]2[C:34]([CH:35]=[CH:36][C:37]([S:41](Cl)(=[O:43])=[O:42])=[CH:38]2)=[CH:33][CH:32]=1.C(=O)([O-])[O-].[Na+].[Na+]>CO.C(OCC)(=O)C.C(N(CC)CC)C.ClCCl>[CH3:29][O:30][C:31]1[CH:40]=[C:39]2[C:34]([CH:35]=[CH:36][C:37]([S:41]([NH:8][C@H:9]3[CH2:13][CH2:12][N:11]([NH:14][CH:15]4[CH2:16][CH2:17][N:18]([C:21]5[CH:22]=[CH:23][N:24]=[CH:25][CH:26]=5)[CH2:19][CH2:20]4)[C:10]3=[O:27])(=[O:43])=[O:42])=[CH:38]2)=[CH:33][CH:32]=1

参加物

9

反応物 4

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 105152667-methoxynaphthalene-2-sulfonyl ChlorideHCID 69545831HCID 69545831、化合物

生成物 1

HCID 69545788HCID 69545788、化合物

試薬・触媒・溶媒 4

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒HCID 8471Triethylamine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of (3S)-3-(tert-butoxycarbonylamino)-1-[1-(4-pyridyl)-4-piperidinylamino]-2-pyrrolidone (220 mg) in methanol (10 ml) was combined with a 4N solution of hydrochloric acid in ethyl acetate (10 ml) and stirred at room temperature for 30 minutes. The reaction mixture was concentrated and the residue obtained was combined with dichloromethane (20 ml) and triethylamine (700 ml), followed by 7-methoxynaphthalene-2-sulfonyl chloride (150 ml) at 0° C., and then stirred at room temperature for 1 hour. The reaction mixture was combined with an aqueous solution of sodium carbonate, extracted with dichloromethane, dried, concentrated and purified by a column chromatography dichloromethane: 10% aqueous ammonia-containing methanol=20:1) to obtain the title compound (123 mg) as a colorless amorphous material.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. customthe residue obtained
  3. stirringstirred at room temperature for 1 hour
  4. extractionextracted with dichloromethane
  5. customdried
  6. concentrationconcentrated
  7. custompurified by a column chromatography dichloromethane
  8. addition10% aqueous ammonia-containing methanol=20:1)

出典と根拠

ORDレコード
ord-9093d822023f4eac817529dd88c436f1
出典データセット
uspto-grants-2004_04
特許番号
US06723722B1

反応ノート

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