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

HRID 471013노트

반응식

HRID 471013 반응식
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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ca4f46956952480d84262dc08730c565
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08629271B2

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