Ammonia → 2-(3-(1-Oxa-4,9-diazaspiro[5.5]undecan-9-ylmethyl)-2-fluorophenyl)ethanol

HRID 1689373

반응식

HRID 1689373 반응식
N.FC(F)(F)C([N:6]1[CH2:11][C:10]2([CH2:16][CH2:15][N:14]([CH2:17][C:18]3[CH:23]=[CH:22][CH:21]=[C:20]([CH2:24][CH2:25][OH:26])[C:19]=3[F:27])[CH2:13][CH2:12]2)[O:9][CH2:8][CH2:7]1)=O>CO>[O:9]1[C:10]2([CH2:16][CH2:15][N:14]([CH2:17][C:18]3[C:19]([F:27])=[C:20]([CH2:24][CH2:25][OH:26])[CH:21]=[CH:22][CH:23]=3)[CH2:13][CH2:12]2)[CH2:11][NH:6][CH2:7][CH2:8]1

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 579893822,2,2-Trifluoro-1-(9-(2-fluoro-3-(2-hydroxyethyl)benzyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)ethanone

생성물 1

HCID 579891872-(3-(1-Oxa-4,9-diazaspiro[5.5]undecan-9-ylmethyl)-2-fluorophenyl)ethanol

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

‘880’ Aqueous ammonia solution (5 mL) was added to a solution of 2,2,2-trifluoro-1-(9-(2-fluoro-3-(2-hydroxyethyl)benzyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)ethanone (example 67, step e) (1.9 g) in methanol (25 mL). The resulting mixture was stirred for 90 min and the solvent evaporated. The residue was purified by silica gel chromatography eluting with 94.5:5:0.5 to 89:10:1 DCM:methanol:‘880’ ammonia gradient. The fractions containing product were combined and evaporated to give a gum that solidified on standing. The white solid was triturated with isohexane and dried over sodium sulphate to give the subtitled compound as a white solid. Yield 1 g.

후처리

  1. customthe solvent evaporated
  2. customThe residue was purified by silica gel chromatography
  3. washeluting with 94.5:5:0.5 to 89:10:1 DCM
  4. additionThe fractions containing product
  5. customevaporated
  6. customto give a gum that
  7. customThe white solid was triturated with isohexane
  8. dry with materialdried over sodium sulphate

출처 및 근거

ORD 기록
ord-42aaa5d94e8a4b079d124b54ccba12c9
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08148373B2

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