Triethylamine → HCID 44159737、化合物

HRID 1886966ノート

反応式

HRID 1886966 の反応式
[NH2:1][CH:2]1[C:8]2=[N:9][C:10]([C:14]3[CH:19]=[CH:18][N:17]=[CH:16][N:15]=3)=[CH:11][C:12](=[O:13])[N:7]2[CH2:6][CH2:5][O:4][CH2:3]1.[C:20]([O:24][C:25]([N:27]1[CH2:36][CH2:35][C:34]2[C:29](=[CH:30][C:31]([C:37](O)=[O:38])=[CH:32][CH:33]=2)[CH2:28]1)=[O:26])([CH3:23])([CH3:22])[CH3:21].C(P(=O)(OCC)OCC)#N.C(N(CC)CC)C>CN(C)C=O.C(OCC)(=O)C.O>[C:20]([O:24][C:25]([N:27]1[CH2:36][CH2:35][C:34]2[C:29](=[CH:30][C:31]([C:37](=[O:38])[NH:1][CH:2]3[C:8]4=[N:9][C:10]([C:14]5[CH:19]=[CH:18][N:17]=[CH:16][N:15]=5)=[CH:11][C:12](=[O:13])[N:7]4[CH2:6][CH2:5][O:4][CH2:3]3)=[CH:32][CH:33]=2)[CH2:28]1)=[O:26])([CH3:23])([CH3:21])[CH3:22]

参加物

8

反応物 4

HCID 8471TriethylamineHCID 76257Diethyl cyanophosphonateHCID 189883742-((Tert-butoxy)carbonyl)-1,2,3,4-tetrahydroisoquinoline-7-carboxylic acidHCID 68626960HCID 68626960、化合物

生成物 1

HCID 44159737HCID 44159737、化合物収率 38.6%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 0.080 g (0.31 mmol) of (+/−)-9-Amino-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-7-oxa-1,4-a-diaza-benzocyclohepten-4-one dissolved in 2.60 mL of dimethylformamide was added 0.086 g (0.31 mmol) of 3,4-dihydro-1H-isoquinoline-2,7-dicarboxylic acid 2-tert-butyl ester. To the resulting mixture was added 60 μL (0.37 mmol) of diethyl cyanophosphonate and 40 μL (0.31 mmol) of triethylamine at 0° C. The resulting mixture was stirred at room temperature for 15 hours. Water and ethyl acetate were added and the mixture was stirred. The resulting residue was filtered, washed with water, ethyl acetate and diethyl ether to afford 0.062 g (38%) of the pure product as a white powder.

後処理

  1. stirringthe mixture was stirred
  2. filtrationThe resulting residue was filtered
  3. washwashed with water, ethyl acetate and diethyl ether

出典と根拠

ORDレコード
ord-073d483f88a04d54866a02d9abd78431
出典データセット
uspto-grants-2013_08
特許番号
US08501728B2

反応ノート

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