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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
ノート
印刷プレビュー

反応式

HRID 1689540 の反応式
[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]
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 84468TrifluoroacetateHCID 579889227,7-Dimethyl-9-oxononyl methanesulfonateHCID 57989152(2-Isopropylthiazol-4-yl)-(1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)methanone

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒
2 回

実験手順

(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.

後処理

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

出典と根拠

ORDレコード
ord-f8d5bfd3855344a99c2f7df2004965c1
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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