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Sodium Hydroxide → HCID 24810337, 화합물

HRID 2081111
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HRID 2081111 반응식
[OH-].[Na+].C([O:5][C:6]([C:8]1[C:9]2[S:17][CH:16]=[C:15]([CH2:18][O:19][C:20]3[CH:25]=[C:24]([C:26]4[O:30][N:29]=[C:28]([CH3:31])[N:27]=4)[CH:23]=[CH:22][C:21]=3[CH3:32])[C:10]=2[C:11]([NH2:14])=[N:12][CH:13]=1)=[O:7])C>O1CCCC1.CO>[NH2:14][C:11]1[C:10]2[C:15]([CH2:18][O:19][C:20]3[CH:25]=[C:24]([C:26]4[O:30][N:29]=[C:28]([CH3:31])[N:27]=4)[CH:23]=[CH:22][C:21]=3[CH3:32])=[CH:16][S:17][C:9]=2[C:8]([C:6]([OH:7])=[O:5])=[CH:13][N:12]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 24810336HCID 24810336, 화합물

생성물 1

HCID 24810337HCID 24810337, 화합물

시약·촉매·용매 1

HCID 21899815MeOH tetrahydrofuran용매

반응 조건

온도
50 °C

실험 절차

An aqueous solution of sodium hydroxide (2 N, 3.0 mL, 1.5 mmol) was added to a solution of 4-amino-3-[2-methyl-5-(3-methyl-[1,2,4]oxadiazol-5-yl)-phenoxymethyl]-thieno[3,2-c]pyridine-7-carboxylic acid ethyl ester (0.33 g, 0.78 mmol) (from Example 54 supra) in tetrahydrofuran/methanol (3:1, 8 mL) and the mixture was heated at 50° C. for 1 day. The reaction mixture was concentrated and azeotroped with toluene. The solid residue was triturated with ethyl acetate. The solid was then suspended in water and treated with hydrochloric acid (1N). After stirring 30 minutes, the solid was collected, washed with water and dried to 4-amino-3-[2-methyl-5-(3-methyl-[1,2,4]oxadiazol-5-yl)-phenoxymethyl]-thieno[3,2-c]pyridine-7-carboxylic acid. (Yield 0.29 g, 94%).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. customazeotroped with toluene
  3. customThe solid residue was triturated with ethyl acetate
  4. additiontreated with hydrochloric acid (1N)
  5. customthe solid was collected
  6. washwashed with water
  7. dry with materialdried to 4-amino-3-[2-methyl-5-(3-methyl-[1,2,4]oxadiazol-5-yl)-phenoxymethyl]-thieno[3,2-c]pyridine-7-carboxylic acid

출처 및 근거

ORD 기록
ord-6660c7c40cb545718147412cdd2c0631
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07932390B2

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