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Trifluoromethanesulfonic anhydride → Trifluoro-methanesulfonic acid 3-cyano-5-methyl-4-(4-phenoxy-phenylamino)-pyrrolo[1,2-b]pyridazin-6-yl ester

HRID 1796636
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HRID 1796636 반응식
[OH:1][C:2]1[C:3]([CH3:27])=[C:4]2[C:9]([NH:10][C:11]3[CH:16]=[CH:15][C:14]([O:17][C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)=[CH:13][CH:12]=3)=[C:8]([C:24]#[N:25])[CH:7]=[N:6][N:5]2[CH:26]=1.[O:28](S(C(F)(F)F)(=O)=O)[S:29]([C:32]([F:35])([F:34])[F:33])(=O)=[O:30]>C(Cl)Cl.CCOC(C)=O>[C:24]([C:8]1[CH:7]=[N:6][N:5]2[CH:26]=[C:2]([O:1][S:29]([C:32]([F:35])([F:34])[F:33])(=[O:30])=[O:28])[C:3]([CH3:27])=[C:4]2[C:9]=1[NH:10][C:11]1[CH:12]=[CH:13][C:14]([O:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[CH:15][CH:16]=1)#[N:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 67749Trifluoromethanesulfonic anhydrideHCID 221796716-Hydroxy-5-methyl-4-(4-phenoxy-phenylamino)-pyrrolo[1,2-b]pyridazine-3-carbonitrile

생성물 1

HCID 86594742Trifluoro-methanesulfonic acid 3-cyano-5-methyl-4-(4-phenoxy-phenylamino)-pyrrolo[1,2-b]pyridazin-6-yl ester수율 95.5%

시약·촉매·용매 2

HCID 6344Dichloromethane용매
HCID 8857
Ethyl Acetate
용매

실험 절차

To a solution of 397A (32 mg, 0.090 mmol) in CH2Cl2 (1 ml) was added Tf2O (18 μl, 0.099 mmol) at −10° C. The reaction mixture was stirred for 5 min, diluted with EtOAc, washed with brine, dried and concentrated to give 397 (42 mg, 95%) LCMS Found: (M+H)+=489.0

후처리

  1. washwashed with brine
  2. customdried
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-7e4fb5160cd7486bbd3d01e95f784e8b
출처 데이터셋
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07030112B2

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