Diisopropylethylamine → 1-(2-Bromo-4,5,7,8-tetrahydro-thiazolo[4,5-d]azepin-6-yl)-2-(5-(4-fluoro-phenyl)-3-p-tolyl-(1,2,4)triazol-1-yl)-ethanone

HRID 239188ノート

反応式

HRID 239188 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]=[C:11]([C:13]3[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=3)[N:10]([CH2:20][C:21](O)=[O:22])[N:9]=2)=[CH:4][CH:3]=1.[CH3:24]CN(C(C)C)C(C)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.[Br:55][C:56]1[S:57][C:58]2[CH2:64][CH2:63][NH:62][CH2:61][CH2:60][C:59]=2[N:65]=1>CN(C=O)C>[Br:55][C:56]1[S:57][C:58]2[CH2:64][CH2:63][N:62]([C:21](=[O:22])[CH2:20][N:10]3[C:11]([C:13]4[CH:14]=[CH:15][C:16]([F:19])=[CH:17][CH:18]=4)=[N:12][C:8]([C:5]4[CH:4]=[CH:3][C:2]([CH3:24])=[CH:7][CH:6]=4)=[N:9]3)[CH2:61][CH2:60][C:59]=2[N:65]=1

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 866864842-Bromo-5,6,7,8-tetrahydro-4H-thiazolo[4,5-d]azepineHCID 86686517(3,5-bis-(4-Fluoro-phenyl)-(1,2,4)triazol-1-yl)-acetic acid

生成物 1

HCID 866865211-(2-Bromo-4,5,7,8-tetrahydro-thiazolo[4,5-d]azepin-6-yl)-2-(5-(4-fluoro-phenyl)-3-p-tolyl-(1,2,4)triazol-1-yl)-ethanone

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

151 mg (3,5-bis-(4-fluoro-phenyl)-(1,2,4)triazol-1-yl)-acetic acid and 84 μL DIPEA were dissolved in 2.5 mL DMF. 154 mg TBTU was added to this solution and the mixture was stirred for 10 min. at RT. Then, 112 mg 2-bromo-5,6,7,8-tetrahydro-4H-thiazolo[4,5-d]azepine in 2.5 mL DMF was added. The mixture was stirred for 2 h at RT. The reaction-solution was purified by HPLC to yield 19.8 mg of the desired compound. Rt: 2.21 (method I), (M+H)+: 530/32

後処理

  1. stirringThe mixture was stirred for 2 h at RT
  2. customThe reaction-solution was purified by HPLC

出典と根拠

ORDレコード
ord-8ace7d62387b47c3b11c4db2425f4cdf
出典データセット
uspto-grants-2014_02
特許番号
US08642774B2

反応ノート

読み込み中…