Triethylamine → 2-Methylpentane

HRID 1689302노트

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HRID 1689302 반응식
CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[C:25]([C:29]1[S:30][CH:31]=[C:32]([C:34]([OH:36])=O)[N:33]=1)([CH3:28])([CH3:27])[CH3:26].[Si:37]([O:44][CH2:45][CH2:46][C:47]1[CH:48]=[C:49]([CH2:52][N:53]2[CH2:63][CH2:62][C:56]3([O:61][CH2:60][CH2:59][NH:58][CH2:57]3)[CH2:55][CH2:54]2)[S:50][CH:51]=1)([C:40]([CH3:43])([CH3:42])[CH3:41])([CH3:39])[CH3:38].C(N(CC)CC)C>CN(C=O)C>[CH3:52][CH2:49][CH2:48][CH:47]([CH3:51])[CH3:46].[Si:37]([O:44][CH2:45][CH2:46][C:47]1[CH:48]=[C:49]([CH2:52][N:53]2[CH2:63][CH2:62][C:56]3([O:61][CH2:60][CH2:59][N:58]([C:34]([C:32]4[N:33]=[C:29]([C:25]([CH3:26])([CH3:27])[CH3:28])[S:30][CH:31]=4)=[O:36])[CH2:57]3)[CH2:55][CH2:54]2)[S:50][CH:51]=1)([C:40]([CH3:41])([CH3:42])[CH3:43])([CH3:39])[CH3:38]

참가 물질

7

반응물 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 288755552-Tert-butyl-1,3-thiazole-4-carboxylic acidHCID 579891139-((4-(2-(tert-Butyldimethylsilyloxy)ethyl)thiophen-2-yl)methyl)-1-oxa-4,9-diazaspiro[5.5]undecane

생성물 2

HCID 78922-MethylpentaneHCID 57989351(9-((4-(2-(Tert-butyldimethylsilyloxy)ethyl)thiophen-2-yl)methyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)(2-tert-butylthiazol-4-yl)methanone

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

HATU (0.306 g) was added to stirred solution of 2-tert-butylthiazole-4-carboxylic acid (0.16 g), 9-((4-(2-(tert-butyldimethylsilyloxy)ethyl)thiophen-2-yl)methyl)-1-oxa-4,9-diazaspiro[5.5]undecane (example 43, step b) (0.300 g) and triethylamine (0.41 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 and brine, dried over magnesium sulphate, filtered and evaporated in vacuo. Purification by silica gel chromatography eluting with ethyl acetate:isohexane:triethylamine, 12:90:10 gave the subtitled compound as a gum. Yield 0.3 g.

후처리

  1. customthe reaction mixture was partitioned between water and ethyl acetate
  2. washThe ethyl acetate layer was washed twice with water and 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

출처 및 근거

ORD 기록
ord-c229df6f9157479f9a4c0a52443dfe5f
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08148373B2

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