Lithium Hydroxide → HCID 178524360, 화합물

HRID 1819482노트

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HRID 1819482 반응식
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]

참가 물질

5

반응물 2

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

생성물 1

HCID 178524360HCID 178524360, 화합물수율 30%

시약·촉매·용매 2

HCID 962Water촉매HCID 887Methanol용매

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온도
50 °C

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-26d6b13705e84d278b7e9b2807522777
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07601714B2

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