Lithium Hydroxide → HCID 178524360、化合物

HRID 1819482ノート

反応式

HRID 1819482 の反応式
C[O:2][C:3](=[O:42])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH2:10][NH:11][CH:12]2[CH2:17][CH2:16][CH:15]([CH2:18][NH:19][C:20]3[C:25]([N+:26]([O-:28])=[O:27])=[CH:24][N:23]=[C:22]([NH:29][CH2:30][C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=4[O:37][C:38]([F:41])([F:40])[F:39])[N:21]=3)[CH2:14][CH2:13]2)[CH:5]=1.[Li+].[OH-]>O.CO>[N+:26]([C:25]1[C:20]([NH:19][CH2:18][C@H:15]2[CH2:16][CH2:17][C@H:12]([NH:11][CH2:10][C:6]3[CH:5]=[C:4]([CH:9]=[CH:8][CH:7]=3)[C:3]([OH:42])=[O:2])[CH2:13][CH2:14]2)=[N:21][C:22]([NH:29][CH2:30][C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=2[O:37][C:38]([F:41])([F:40])[F:39])=[N:23][CH:24]=1)([O-:28])=[O:27]

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 598456853-[(4-{[5-Nitro-2-(2-trifluoromethoxy-benzylamino)-pyrimidin-4-ylamino]-methyl}-cyclohexylamino)-methyl]-benzoic acid methyl ester

生成物 1

HCID 178524360HCID 178524360、化合物収率 30%

試薬・触媒・溶媒 2

HCID 962Water触媒HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

A mixture of 3-[(4-{[5-nitro-2-(2-trifluoromethoxy-benzylamino)-pyrimidin-4-ylamino]-methyl}-cyclohexylamino)-methyl]-benzoic acid methyl ester (75 mg, 0.13 mmol), LiOH (30 mg, 1.29 mmol) and water (3 drops) in MeOH (2 mL) was heated at 50° C. for 18 h. The reaction mixture was concentrated in vacuo then taken up in water and EtOAc. Dilute HCl was added until the aqueous phase reached pH 6. The solid that precipitated was isolated by filtration to afford the target compound (20 mg, 30%) as a white solid, m/z 575 (M+1)+.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. additionDilute HCl was added until the aqueous phase
  3. customThe solid that precipitated
  4. customwas isolated by filtration

出典と根拠

ORDレコード
ord-26d6b13705e84d278b7e9b2807522777
出典データセット
uspto-grants-2009_10
特許番号
US07601714B2

反応ノート

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