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Triethylamine → (9-(2-Fluoro-3-(2-hydroxyethyl)benzyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)(2-(2,2,2-trifluoroethyl)thiazol-4-yl)methanone

HRID 1689374
ノート
印刷プレビュー

反応式

HRID 1689374 の反応式
CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[F:25][C:26]([F:37])([F:36])[CH2:27][C:28]1[S:29][CH:30]=[C:31]([C:33]([OH:35])=O)[N:32]=1.[O:38]1[C:43]2([CH2:48][CH2:47][N:46]([CH2:49][C:50]3[C:51]([F:59])=[C:52]([CH2:56][CH2:57][OH:58])[CH:53]=[CH:54][CH:55]=3)[CH2:45][CH2:44]2)[CH2:42][NH:41][CH2:40][CH2:39]1.C(N(CC)CC)C>CN(C=O)C>[F:59][C:51]1[C:52]([CH2:56][CH2:57][OH:58])=[CH:53][CH:54]=[CH:55][C:50]=1[CH2:49][N:46]1[CH2:47][CH2:48][C:43]2([O:38][CH2:39][CH2:40][N:41]([C:33]([C:31]3[N:32]=[C:28]([CH2:27][C:26]([F:25])([F:37])[F:36])[S:29][CH:30]=3)=[O:35])[CH2:42]2)[CH2:44][CH2:45]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 579889492-(2,2,2-Trifluoroethyl)-1,3-thiazole-4-carboxylic acidHCID 579891872-(3-(1-Oxa-4,9-diazaspiro[5.5]undecan-9-ylmethyl)-2-fluorophenyl)ethanol

生成物 1

HCID 57989017
(9-(2-Fluoro-3-(2-hydroxyethyl)benzyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)(2-(2,2,2-trifluoroethyl)thiazol-4-yl)methanone

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

HATU (0.181 g) was added in one portion to a stirred solution at 0° C. of 2-(2,2,2-trifluoroethyl)thiazole-4-carboxylic acid (example 67, step d) (0.077 g) and 2-(3-(1-oxa-4,9-diazaspiro[5.5]undecan-9-ylmethyl)-2-fluorophenyl)ethanol (example 67, step f) (0.113 g) and triethylamine (0.153 mL) in DMF (5 mL). The reaction mixture was stirred at room temperature for 2 hours. The mixture was partitioned between ethyl acetate and brine, the organic layer was washed twice with brine, dried over sodium sulphate, filtered and the solvent evaporated under reduced pressure to afford the subtitled compound. Yield 0.180 g.

後処理

  1. customThe mixture was partitioned between ethyl acetate and brine
  2. washthe organic layer was washed twice with brine
  3. dry with materialdried over sodium sulphate
  4. filtrationfiltered
  5. customthe solvent evaporated under reduced pressure

出典と根拠

ORDレコード
ord-54d093387a124a93860cecf2025ba0d5
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08148373B2

反応ノート

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