Methanol → HCID 178474871, 화합물

HRID 1373137노트

반응식

HRID 1373137 반응식
C([N:4]1[C:12]2[C:7](=[CH:8][C:9]([N:13](C(=O)C)[S:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)(=[O:16])=[O:15])=[CH:10][CH:11]=2)[C:6](=[C:26](OCC)[C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:5]1=[O:36])(=O)C.[C:37]([N:40]([C:50]1[CH:56]=[CH:55][C:53]([NH2:54])=[CH:52][CH:51]=1)[CH2:41][CH2:42][NH:43]C(=O)C(F)(F)F)(=[O:39])[CH3:38].CO.[OH-].[Na+]>CN(C=O)C.O>[C:37]([N:40]([C:50]1[CH:51]=[CH:52][C:53]([NH:54]/[C:26](=[C:6]2\[C:5](=[O:36])[NH:4][C:12]3[C:7]\2=[CH:8][C:9]([NH:13][S:14]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)(=[O:16])=[O:15])=[CH:10][CH:11]=3)/[C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)=[CH:55][CH:56]=1)[CH2:41][CH2:42][NH2:43])(=[O:39])[CH3:38]

참가 물질

7

반응물 4

HCID 887MethanolHCID 14798Sodium HydroxideHCID 120470014-[N-acetyl-N-(2-trifluoroacetylamino-ethyl)-amino]-anilineHCID 695098291-acetyl-3-(1-ethoxy-1-phenyl-methylidene)-5-(N-acetyl-N-phenylsulphonyl-amino)-2-indolinone

생성물 1

HCID 178474871HCID 178474871, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A mixture of 0.5 g (1 mmol) of 1-acetyl-3-(1-ethoxy-1-phenyl-methylidene)-5-(N-acetyl-N-phenylsulphonyl-amino)-2-indolinone and 0.3 g (1.2 mmol) of 4-[N-acetyl-N-(2-trifluoroacetylamino-ethyl)-amino]-aniline are stirred in 5 ml of DMF for 6 hours at 120° C. After cooling to ambient temperature 5 ml of methanol and 3 ml (6 mmol) of 2 N sodium hydroxide solution are added, and the mixture is stirred for 30 minutes. The reaction mixture is diluted with 50 ml of water and the crystalline precipitate is suction filtered and dried. The residue is chromatographed on silica gel (dichloromethane/methanol/ammonia=9:1:0.1).

후처리

  1. additionare added
  2. filtrationfiltered
  3. customdried
  4. customThe residue is chromatographed on silica gel (dichloromethane/methanol/ammonia=9:1:0.1)

출처 및 근거

ORD 기록
ord-d7577033038f420bb8ac47a0ca3e5739
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07160901B2

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