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Water → 2-[[7-[[Dimethyl(oxo)-lambda6-sulfanylidene]amino]-5-methyl-quinazolin-4-yl]amino]-5-fluoro-phenol

HRID 1396651
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HRID 1396651 반응식
C([O:8][C:9]1[CH:14]=[C:13]([F:15])[CH:12]=[CH:11][C:10]=1[NH:16][C:17]1[C:26]2[C:21](=[CH:22][C:23]([N:28]=[S:29]([CH3:32])([CH3:31])=[O:30])=[CH:24][C:25]=2[CH3:27])[N:20]=[CH:19][N:18]=1)C1C=CC=CC=1.B(Br)(Br)Br.O>C(Cl)Cl>[CH3:32][S:29](=[N:28][C:23]1[CH:22]=[C:21]2[C:26]([C:17]([NH:16][C:10]3[CH:11]=[CH:12][C:13]([F:15])=[CH:14][C:9]=3[OH:8])=[N:18][CH:19]=[N:20]2)=[C:25]([CH3:27])[CH:24]=1)([CH3:31])=[O:30]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 25134Boron tribromideHCID 86718469N-(2-benzyloxy-4-fluoro-phenyl)-7-[[dimethyl(oxo)-lambda6-sulfanylidene]amino]-5-methyl-quinazolin-4-amine

생성물 1

HCID 867184712-[[7-[[Dimethyl(oxo)-lambda6-sulfanylidene]amino]-5-methyl-quinazolin-4-yl]amino]-5-fluoro-phenol

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3.5 g (7.8 mmol) of N-(2-benzyloxy-4-fluoro-phenyl)-7-[[dimethyl(oxo)-λ6-sulfanylidene]amino]-5-methyl-quinazolin-4-amine in DCM are cooled to 0° C., 0.9 ml (9.3 mmol) boron tribromide are added dropwise and the reaction mixture is stirred for 15 min. Water is added cautiously and the aqueous layer is separated and extracted with DCM. The organic phases are pooled, washed with water, dried and evaporated. The residue is treated with isopropanol, filtered and dried.

후처리

  1. customthe aqueous layer is separated
  2. extractionextracted with DCM
  3. washwashed with water
  4. customdried
  5. customevaporated
  6. additionThe residue is treated with isopropanol
  7. filtrationfiltered
  8. customdried

출처 및 근거

ORD 기록
ord-fb0d626ec6fd43b18ed4ac4e8b1c6013
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08901138B2

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