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Pyridine → 3-n-Butylaminocarbonyloxy-2-(7-chloro-1,8-naphthyridin-2-yl)-5-trifluoromethyl-isoindolin-1-one

HRID 2083743
ノート
印刷プレビュー

反応式

HRID 2083743 の反応式
N1C=CC=CC=1.[CH2:7]([N:11]=[C:12]=[O:13])[CH2:8][CH2:9][CH3:10].[Cl:14][C:15]1[N:24]=[C:23]2[C:18]([CH:19]=[CH:20][C:21]([N:25]3[CH:33]([OH:34])[C:32]4[C:27](=[CH:28][CH:29]=[C:30]([C:35]([F:38])([F:37])[F:36])[CH:31]=4)[C:26]3=[O:39])=[N:22]2)=[CH:17][CH:16]=1.C(N(CC)CC)C>C(#N)C>[CH2:7]([NH:11][C:12]([O:34][CH:33]1[C:32]2[C:27](=[CH:28][CH:29]=[C:30]([C:35]([F:37])([F:38])[F:36])[CH:31]=2)[C:26](=[O:39])[N:25]1[C:21]1[CH:20]=[CH:19][C:18]2[C:23](=[N:24][C:15]([Cl:14])=[CH:16][CH:17]=2)[N:22]=1)=[O:13])[CH2:8][CH2:9][CH3:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 1049PyridineHCID 8110Butyl isocyanateHCID 8471TriethylamineHCID 227547132-(7-Chloro-1,8-naphthyridin-2-yl)-3-hydroxy-5-trifluoromethyl-isoindolin-1-one

生成物 1

HCID 227547593-n-Butylaminocarbonyloxy-2-(7-chloro-1,8-naphthyridin-2-yl)-5-trifluoromethyl-isoindolin-1-one

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒

実験手順

Pyridine (10 cc.) and n-butyl isocyanate (11.2 cc.) are added to a suspension of 2-(7-chloro-1,8-naphthyridin-2-yl)-3-hydroxy-5-trifluoromethyl-isoindolin-1-one (3.8 g.) in acetonitrile (380 cc.). The mixture is heated to the reflux temperature and triethylamine (0.5 cc.) is then added. Refluxing is continued for 1 hour and 30 minutes until dissolution. The reaction mixture is then concentrated under reduced pressure (40 mm.Hg), and the residue is recrystallised from acetonitrile (48 cc.) to give 3-n-butylaminocarbonyloxy-2-(7-chloro-1,8-naphthyridin-2-yl)-5-trifluoromethyl-isoindolin-1-one (3.5 g.) melting at 120° C. and then at 176° C.

後処理

  1. additionis then added
  2. temperatureRefluxing
  3. dissolutionis continued for 1 hour and 30 minutes until dissolution
  4. concentrationThe reaction mixture is then concentrated under reduced pressure (40 mm.Hg)
  5. customthe residue is recrystallised from acetonitrile (48 cc.)

出典と根拠

ORDレコード
ord-c745893c0cbb43b6bf03281ee43b0298
出典データセット
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04086348

反応ノート

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