Ammonia → 9-(3-(2-(tert-Butyldimethylsilyloxy)ethyl)-2-fluorobenzyl)-1-oxa-4,9-diazaspiro[5.5]undecane

HRID 471173ノート

反応式

HRID 471173 の反応式
N.[Si:2]([O:9][CH2:10][CH2:11][C:12]1[C:13]([F:36])=[C:14]([CH:33]=[CH:34][CH:35]=1)[CH2:15][N:16]1[CH2:32][CH2:31][C:19]2([O:24][CH2:23][CH2:22][N:21](C(=O)C(F)(F)F)[CH2:20]2)[CH2:18][CH2:17]1)([C:5]([CH3:8])([CH3:7])[CH3:6])([CH3:4])[CH3:3]>CO>[Si:2]([O:9][CH2:10][CH2:11][C:12]1[C:13]([F:36])=[C:14]([CH:33]=[CH:34][CH:35]=1)[CH2:15][N:16]1[CH2:17][CH2:18][C:19]2([O:24][CH2:23][CH2:22][NH:21][CH2:20]2)[CH2:31][CH2:32]1)([C:5]([CH3:8])([CH3:6])[CH3:7])([CH3:4])[CH3:3]

参加物

4

反応物 2

HCID 222AmmoniaHCID 579890151-(9-(3-(2-(tert-Butyldimethylsilyloxy)ethyl)-2-fluorobenzyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)-2,2,2-trifluoroethanone

生成物 1

HCID 579891399-(3-(2-(tert-Butyldimethylsilyloxy)ethyl)-2-fluorobenzyl)-1-oxa-4,9-diazaspiro[5.5]undecane

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

‘880’ Aqueous ammonia (3.0 mL) was added to stirred solution of 1-(9-(3-(2-(tert-butyldimethylsilyloxy)ethyl)-2-fluorobenzyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)-2,2,2-trifluoroethanone (example 78, step c) (2.5 g) in MeOH (10 mL). After 1 h, the reaction mixture was evaporated to dryness. Acetonitrile was added, the solution was evaporated to dryness in vacuo, and the process repeated three times to give the subtitled compound as an oil. Yield 2.07 g. Used directly.

後処理

  1. customthe reaction mixture was evaporated to dryness
  2. additionAcetonitrile was added
  3. customthe solution was evaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-3b41524af0df49c98ad1da54e9568f5c
出典データセット
uspto-grants-2014_01
特許番号
US08629271B2

反応ノート

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