Formic Acid → 3-(2-(4-(5-Methylthiophene-2-carbonyl)-1-oxa-4,9-diazaspiro[5,5]undecan-9-yl)-ethyl)benzaldehyde

HRID 1689244ノート

反応式

HRID 1689244 の反応式
C(O)=O.C([O:6][CH:7](OCC)[C:8]1[CH:9]=[C:10]([CH:32]=[CH:33][CH:34]=1)[CH2:11][CH2:12][N:13]1[CH2:31][CH2:30][C:16]2([O:21][CH2:20][CH2:19][N:18]([C:22]([C:24]3[S:25][C:26]([CH3:29])=[CH:27][CH:28]=3)=[O:23])[CH2:17]2)[CH2:15][CH2:14]1)C>O1CCCC1.O>[CH3:29][C:26]1[S:25][C:24]([C:22]([N:18]2[CH2:17][C:16]3([CH2:30][CH2:31][N:13]([CH2:12][CH2:11][C:10]4[CH:9]=[C:8]([CH:34]=[CH:33][CH:32]=4)[CH:7]=[O:6])[CH2:14][CH2:15]3)[O:21][CH2:20][CH2:19]2)=[O:23])=[CH:28][CH:27]=1

参加物

5

反応物 2

HCID 284Formic AcidHCID 57988993(9-(3-(Diethoxymethyl)phenethyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)(5-methylthiophen-2-yl)methanone

生成物 1

HCID 579893523-(2-(4-(5-Methylthiophene-2-carbonyl)-1-oxa-4,9-diazaspiro[5,5]undecan-9-yl)-ethyl)benzaldehyde

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Formic acid (2 mL) was added to stirred solution of (9-(3-(diethoxymethyl)phenethyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)(5-methylthiophen-2-yl)methanone (example 20, step e) (0.20 g) in tetrahydrofuran (3 mL) and water (1 mL) cooled in an ice bath. After 10 min, the reaction mixture was evaporated in vacuo, toluene was added and the reaction mixture was evaporated in vacuo. The residue was dissolved in acetonitrile and then evaporated in vacuo, and this process was repeated to give the subtitled compound as an oil that was used directly. Yield 0.16 g.

後処理

  1. temperaturecooled in an ice bath
  2. customthe reaction mixture was evaporated in vacuo, toluene
  3. additionwas added
  4. customthe reaction mixture was evaporated in vacuo
  5. dissolutionThe residue was dissolved in acetonitrile
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-7f9789368caf4c4e95ab21d5fa1b8872
出典データセット
uspto-grants-2012_04
特許番号
US08148373B2

反応ノート

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