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Triethylamine → 9-(4-(2-Isopropylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)-3,3-dimethylnonanal

HRID 1689540
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HRID 1689540 반응식
[CH:1]([C:4]1[S:5][CH:6]=[C:7]([C:9]([N:11]2[CH2:16][C:15]3([CH2:21][CH2:20][NH:19][CH2:18][CH2:17]3)[O:14][CH2:13][CH2:12]2)=[O:10])[N:8]=1)([CH3:3])[CH3:2].FC(F)(F)C([O-])=O.C(N(CC)CC)C.CS(O[CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][C:47]([CH3:52])([CH3:51])[CH2:48][CH:49]=[O:50])(=O)=O>C(#N)C>[CH:1]([C:4]1[S:5][CH:6]=[C:7]([C:9]([N:11]2[CH2:16][C:15]3([CH2:17][CH2:18][N:19]([CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][C:47]([CH3:51])([CH3:52])[CH2:48][CH:49]=[O:50])[CH2:20][CH2:21]3)[O:14][CH2:13][CH2:12]2)=[O:10])[N:8]=1)([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 84468TrifluoroacetateHCID 579889227,7-Dimethyl-9-oxononyl methanesulfonateHCID 57989152(2-Isopropylthiazol-4-yl)-(1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)methanone

생성물 1

HCID 579893649-(4-(2-Isopropylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)-3,3-dimethylnonanal

시약·촉매·용매 1

HCID 6342
Acetonitrile
용매
2회

실험 절차

(2-Isopropyl-thiazol-4-yl)-(1-oxa-4,9-diaza-spiro[5.5]undec-4-yl)-methanone (0.262 g) (prepared from the trifluoroacetate salt as in Example 102, step c) was dissolved in acetonitrile (4 mL) and triethylamine (0.22 mL) was added. This solution was then added to a solution of 7,7-dimethyl-9-oxononyl methanesulfonate (Example 279, step e) (0.291 g) in acetonitrile (4 mL) and the resultant mixture heated at 80° C. overnight. The solvents were removed under vacuum. Purification was by silica gel chromatography eluting with 0-10% Methanol in DCM to afford the subtitled compound as a colourless oil. Yield 0.361 g.

후처리

  1. customThe solvents were removed under vacuum
  2. customPurification
  3. washeluting with 0-10% Methanol in DCM

출처 및 근거

ORD 기록
ord-f8d5bfd3855344a99c2f7df2004965c1
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08148373B2

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