Triethylamine → HCID 59175839、化合物

HRID 1807782ノート

反応式

HRID 1807782 の反応式
[CH:1]1([CH2:4][NH:5][C:6](=[O:17])[NH:7][C:8]2[CH:16]=[CH:15][C:11]([C:12]([OH:14])=O)=[CH:10][CH:9]=2)[CH2:3][CH2:2]1.[F:18][C:19]([F:41])([F:40])[C:20]([C:26]1[CH:39]=[CH:38][C:29]([CH2:30][N:31]2[CH2:36][CH2:35][NH:34][CH2:33][C:32]2=[O:37])=[CH:28][CH:27]=1)([OH:25])[C:21]([F:24])([F:23])[F:22].C(N(CC)CC)C.CCCP1(OP(CCC)(=O)OP(CCC)(=O)O1)=O>ClCCl>[CH:1]1([CH2:4][NH:5][C:6]([NH:7][C:8]2[CH:9]=[CH:10][C:11]([C:12]([N:34]3[CH2:35][CH2:36][N:31]([CH2:30][C:29]4[CH:38]=[CH:39][C:26]([C:20]([OH:25])([C:19]([F:18])([F:40])[F:41])[C:21]([F:24])([F:22])[F:23])=[CH:27][CH:28]=4)[C:32](=[O:37])[CH2:33]3)=[O:14])=[CH:15][CH:16]=2)=[O:17])[CH2:2][CH2:3]1

参加物

6

反応物 4

HCID 8471TriethylamineHCID 111923Propylphosphonic anhydrideHCID 580558194-(3-(Cyclopropylmethyl)ureido)benzoic acidHCID 86638571HCID 86638571、化合物

生成物 1

HCID 59175839HCID 59175839、化合物収率 22.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a stirring solution of 4-(3-(cyclopropylmethyl)ureido)benzoic acid (0.337 mmol, 79 mg), 1-(4-(1,1,1,3,3,3-hexafluoro-2-hydroxypropan-2-yl)benzyl)piperazin-2-one (0.281 mmol, 100 mg) and triethylamine (0.842 mmol, 85 mg) in dichloromethane (10 ml) was added 1-propanephosphonic acid cyclic anhydride (0.421 mmol, 268 mg; 50% solution in ethyl acetate). The reaction mixture was stirred at room temperature for 2 hours. The reaction mixture was diluted with dichloromethane (20 mL) and washed with saturated aqueous sodium hydrogen carbonate solution (30 mL). The organic phase was concentrated and the resulting residue was purified by column chromatography on silica gel (eluting with 5% methanol/95% dichloromethane) to afford the title compound (36 mg). MS (ESI) m/z 573.0 [M+H]+

後処理

  1. washwashed with saturated aqueous sodium hydrogen carbonate solution (30 mL)
  2. concentrationThe organic phase was concentrated
  3. customthe resulting residue was purified by column chromatography on silica gel (eluting with 5% methanol/95% dichloromethane)

出典と根拠

ORDレコード
ord-17937476791e4218aeb927f1ad51d801
出典データセット
uspto-grants-2013_01
特許番号
US08357679B2

反応ノート

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