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Triethylamine → 2-Methylpentane

HRID 471093
ノート
印刷プレビュー

反応式

HRID 471093 の反応式
CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH3:25][C:26]1[S:27][C:28]2[CH:34]=[CH:33][C:32]([C:35]([OH:37])=O)=[CH:31][C:29]=2[N:30]=1.[Si:38]([O:45][CH2:46][CH2:47][C:48]1[CH:49]=[C:50]([CH2:53][N:54]2[CH2:64][CH2:63][C:57]3([O:62][CH2:61][CH2:60][NH:59][CH2:58]3)[CH2:56][CH2:55]2)[S:51][CH:52]=1)([C:41]([CH3:44])([CH3:43])[CH3:42])([CH3:40])[CH3:39].C(N(CC)CC)C>CN(C=O)C>[CH3:28][CH2:29][CH2:31][CH:32]([CH3:35])[CH3:33].[Si:38]([O:45][CH2:46][CH2:47][C:48]1[CH:49]=[C:50]([CH2:53][N:54]2[CH2:64][CH2:63][C:57]3([O:62][CH2:61][CH2:60][N:59]([C:35]([C:32]4[CH:33]=[CH:34][C:28]5[S:27][C:26]([CH3:25])=[N:30][C:29]=5[CH:31]=4)=[O:37])[CH2:58]3)[CH2:56][CH2:55]2)[S:51][CH:52]=1)([C:41]([CH3:42])([CH3:43])[CH3:44])([CH3:40])[CH3:39]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 6499532-Methyl-1,3-benzothiazole-5-carboxylic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 579891139-((4-(2-(tert-Butyldimethylsilyloxy)ethyl)thiophen-2-yl)methyl)-1-oxa-4,9-diazaspiro[5.5]undecane

生成物 2

HCID 78922-Methylpentane
HCID 57989353
(9-((4-(2-(Tert-butyldimethylsilyloxy)ethyl)thiophen-2-yl)methyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)(2-methylbenzo[d]thiazol-5-yl)methanone

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

HATU (0.333 g) was added to stirred solution of 2-methylbenzo[d]thiazole-5-carboxylic acid (0.17 g), 9-((4-(2-(tert-butyldimethylsilyloxy)ethyl)thiophen-2-yl)methyl)-1-oxa-4,9-diazaspiro[5.5]undecane (example 43, step b) (0.3 g) and triethylamine (0.407 mL) in DMF (3 mL). After 1 h, the reaction mixture was partitioned between water and ethyl acetate. The ethyl acetate layer was washed twice with water, once with brine, dried over magnesium sulphate, filtered and evaporated in vacuo. Purification by silica gel chromatography eluting with ethyl acetate:isohexane:triethylamine, 2:8:1 gave the subtitled compound as a gum. Yield 0.36 g.

後処理

  1. customthe reaction mixture was partitioned between water and ethyl acetate
  2. washThe ethyl acetate layer was washed twice with water, once with brine
  3. dry with materialdried over magnesium sulphate
  4. filtrationfiltered
  5. customevaporated in vacuo
  6. customPurification by silica gel chromatography
  7. washeluting with ethyl acetate

出典と根拠

ORDレコード
ord-9a8f087a66bc49038e372dd3062a1b28
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08629271B2

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