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Triethylamine → 4-[N-[1-[N-(benzofuran-2-ylcarbonyl)amino]cyclohexanecarbonyl]amino]-1-[2-(3,3-dimethylazetidin-2-one-1-yl)phenyl]piperidin-3-one

HRID 1392391
ノート
印刷プレビュー

反応式

HRID 1392391 の反応式
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[CH:3]=[C:2]1[C:10]([NH:12][C:13]1([C:19]([NH:21][CH:22]2[CH2:27][CH2:26][N:25]([C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=3[N:34]3[CH2:37][C:36]([CH3:39])([CH3:38])[C:35]3=[O:40])[CH2:24][CH:23]2[OH:41])=[O:20])[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1)=[O:11].C(N(CC)CC)C>CS(C)=O.C(OCC)(=O)C>[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[CH:3]=[C:2]1[C:10]([NH:12][C:13]1([C:19]([NH:21][CH:22]2[CH2:27][CH2:26][N:25]([C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=3[N:34]3[CH2:37][C:36]([CH3:38])([CH3:39])[C:35]3=[O:40])[CH2:24][C:23]2=[O:41])=[O:20])[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1)=[O:11]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 8471TriethylamineHCID 693118614-[N-[1-[N-(benzofuran-2-ylcarbonyl)amino]cyclohexanecarbonyl]amino]-1-[2-(3,3-dimethylazetidin-2-one-1-yl)phenyl]piperidin-3-ol

生成物 1

HCID 104377104-[N-[1-[N-(benzofuran-2-ylcarbonyl)amino]cyclohexanecarbonyl]amino]-1-[2-(3,3-dimethylazetidin-2-one-1-yl)phenyl]piperidin-3-one収率 86%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒
HCID 8857
Ethyl Acetate
溶媒

反応条件

温度
0 °C

実験手順

To the solution of 4-[N-[1-[N-(benzofuran-2-ylcarbonyl)amino]cyclohexanecarbonyl]amino]-1-[2-(3,3-dimethylazetidin-2-one-1-yl)phenyl]piperidin-3-ol (0.14 g) obtained in Step 4 in 3 ml of dimethylsulfoxide (DMSO), was added 0.16 ml of triethylamine. The reaction mixture was cooled to 0° C. Pyridine-SO3 complex (0.15 g) was added slowly to the reaction mixture, which was stirred for about 10 hours at room temperature. The reaction mixture was diluted with 20 ml of ethyl acetate, washed with brine. The resulting organic layer was dried and concentrated on sodium sulfate. The resulting residue was filtered and dried to give 120 mg of the titled compound as white color.

後処理

  1. additionPyridine-SO3 complex (0.15 g) was added slowly to the reaction mixture, which
  2. washwashed with brine
  3. customThe resulting organic layer was dried
  4. concentrationconcentrated on sodium sulfate
  5. filtrationThe resulting residue was filtered
  6. customdried

出典と根拠

ORDレコード
ord-4a51d1f997714eab9e8d3039d5ee1ab8
出典データセット
uspto-grants-2008_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07342027B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート