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Methylamine → HCID 24877276、化合物

HRID 2196175
ノート
印刷プレビュー

反応式

HRID 2196175 の反応式
[CH3:1][C:2]1([CH3:33])[O:6]/[C:5](=[C:7]2/[C:8](=[O:26])[NH:9][C:10]3[C:15]/2=[CH:14][CH:13]=[C:12]([S:16][C:17]2[CH:25]=[CH:24][CH:23]=[CH:22][C:18]=2[C:19](O)=[O:20])[CH:11]=3)/[CH:4]=[C:3]1[N:27]1[CH2:32][CH2:31][O:30][CH2:29][CH2:28]1.CN.C1COCC1.[CH3:41][N:42](C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C>CN(C=O)C.O>[CH3:33][C:2]1([CH3:1])[O:6]/[C:5](=[C:7]2/[C:8](=[O:26])[NH:9][C:10]3[C:15]/2=[CH:14][CH:13]=[C:12]([S:16][C:17]2[CH:25]=[CH:24][CH:23]=[CH:22][C:18]=2[C:19]([NH:42][CH3:41])=[O:20])[CH:11]=3)/[CH:4]=[C:3]1[N:27]1[CH2:32][CH2:31][O:30][CH2:29][CH2:28]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 6329MethylamineHCID 8028TetrahydrofuranHCID 81531DiisopropylethylamineHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 24877383HCID 24877383、化合物

生成物 1

HCID 24877276HCID 24877276、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a stirred solution of 2-{[(3E)-3-(5,5-dimethyl-4-morpholin-4-ylfuran-2(5H)-ylidene)-2-oxo-2,3-dihydro-1H-indol-6-yl]thio}benzoic acid in 5 mL of anhydrous DMF, were added 2M methylamine in THF solution (0.066 mL, 0.13 mmol), HBTU (49 mg, 0.13 mmol) and DIPEA (31 mg, 0.24 mmol). The reaction mixture was stirred at room temperature for 15 minutes and poured into 100 mL of water. The precipitates were filtered, washed with water and dried to give the crude product as a brown solid. Purification of the crude product by silica gel chromatography eluted with a gradient of 5-15% MeOH in CHCl3 afforded 2-{[(3E)-3-(5,5-dimethyl-4-morpholin-4-ylfuran-2(5H)-ylidene)-2-oxo-2,3-dihydro-1H-indol-6-yl]thio}-N-methylbenzamide as brown solid. Yield: 6 mg, 12%.

後処理

  1. filtrationThe precipitates were filtered
  2. washwashed with water
  3. customdried
  4. customto give the crude product as a brown solid
  5. customPurification of the crude product by silica gel chromatography
  6. washeluted with a gradient of 5-15% MeOH in CHCl3

出典と根拠

ORDレコード
ord-4e9993ef2adf4588a27fa0e8972b595d
出典データセット
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08338415B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート