HCID 52933910、化合物 → HCID 52934135、化合物

HRID 1024477ノート

反応式

HRID 1024477 の反応式
[C:1]([C:3]([C:6]1[CH:36]=[CH:35][C:9]([C:10]([NH:12][C:13]2[CH:18]=[CH:17][C:16]([C:19]3[S:23][C:22]([C:24]([NH:26][CH:27]([CH:32]([CH3:34])[CH3:33])[C:28]([O:30]C)=[O:29])=[O:25])=[N:21][CH:20]=3)=[CH:15][CH:14]=2)=[O:11])=[CH:8][CH:7]=1)([CH3:5])[CH3:4])#[N:2]>C1COCC1.CO.O.[OH-].[Li+]>[C:1]([C:3]([C:6]1[CH:36]=[CH:35][C:9]([C:10]([NH:12][C:13]2[CH:14]=[CH:15][C:16]([C:19]3[S:23][C:22]([C:24]([NH:26][CH:27]([CH:32]([CH3:33])[CH3:34])[C:28]([OH:30])=[O:29])=[O:25])=[N:21][CH:20]=3)=[CH:17][CH:18]=2)=[O:11])=[CH:8][CH:7]=1)([CH3:4])[CH3:5])#[N:2]

参加物

5

反応物 1

HCID 52933910HCID 52933910、化合物

生成物 1

HCID 52934135HCID 52934135、化合物

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒HCID 168937Lithium hydroxide, monohydrate溶媒

実験手順

To methyl 2-(5-(4-(4-(2-cyanopropan-2-yl)benzamido)phenyl)thiazole-2-carboxamido)-3-methylbutanoate (Example 85, 65 mg) in THF (1 ml), methanol (1 ml) and 1M lithium hydroxide monohydrate (0.51 ml) was added and reaction mixture was stirred overnight at RT. Organic solvent was concentrated and added water, dilute HCl was added under stirring to pH acidic. The reaction mixture was filtered, to obtain the title compound. Yield: 22 mg (35%). 1HNMR (DMSO-d6, 300 MHz): δ 13.0 (bs, 1H), 10.49 (s, 1H), 8.4 (s, 1H), 8.37 (d, 1H), 8.04 (d, 2H), 7.93 (d, 2H), 7.81 (d, 2H), 7.71 (d, 2H), 4.31 (m, 1H), 2.25 (m, 1H), 1.74 (s, 6H), 0.97 (m, 6H); MS (ES+) m/z 491.2 (M+1).

後処理

  1. customreaction mixture
  2. concentrationOrganic solvent was concentrated
  3. additionadded water, dilute HCl
  4. additionwas added
  5. stirringunder stirring
  6. filtrationThe reaction mixture was filtered

出典と根拠

ORDレコード
ord-7f4be3bdcc0e4a52bfdffa93ced91cef
出典データセット
uspto-grants-2014_05
特許番号
US08722901B2

反応ノート

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