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Triethylamine → (R)-N-(bis(4-methoxyphenyl)(phenyl)methyl)-5-(5-bromo-2-fluorophenyl)-6,6-difluoro-5-methyl-2,5,6,7-tetrahydro-1,4-oxazepin-3-amine

HRID 1186139
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HRID 1186139 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:19])=[C:6]([C@:8]2([CH3:18])[C:14]([F:16])([F:15])[CH2:13][O:12][CH2:11][C:10]([NH2:17])=[N:9]2)[CH:7]=1.CCN(CC)CC.[CH3:27][O:28][C:29]1[CH:34]=[CH:33][C:32]([C:35](Cl)([C:42]2[CH:47]=[CH:46][C:45]([O:48][CH3:49])=[CH:44][CH:43]=2)[C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)=[CH:31][CH:30]=1>ClCCl>[CH3:49][O:48][C:45]1[CH:44]=[CH:43][C:42]([C:35]([C:32]2[CH:31]=[CH:30][C:29]([O:28][CH3:27])=[CH:34][CH:33]=2)([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[NH:17][C:10]2[CH2:11][O:12][CH2:13][C:14]([F:16])([F:15])[C@:8]([C:6]3[CH:7]=[C:2]([Br:1])[CH:3]=[CH:4][C:5]=3[F:19])([CH3:18])[N:9]=2)=[CH:47][CH:46]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 968311,1'-(Chlorophenylmethylene)bis(4-methoxybenzene)HCID 58563049(R)-5-(5-bromo-2-fluorophenyl)-6,6-difluoro-5-methyl-2,5,6,7-tetrahydro-1,4-oxazepin-3-amine

생성물 1

HCID 67468385(R)-N-(bis(4-methoxyphenyl)(phenyl)methyl)-5-(5-bromo-2-fluorophenyl)-6,6-difluoro-5-methyl-2,5,6,7-tetrahydro-1,4-oxazepin-3-amine

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

To a solution of (R)-5-(5-bromo-2-fluorophenyl)-6,6-difluoro-5-methyl-2,5,6,7-tetrahydro-1,4-oxazepin-3-amine (9.0 mmol) in dichloromethane (150 ml) was subsequently added at 0° C. NEt3 (18.0 mmol) and 4,4′-dimethoxytriphenylmethyl chloride (9.9 mmol) and stirring was continued at 22° C. for 2 h. The mixture was washed with saturated aqueous NH4Cl, the organic layer was dried, evaporated and the residue was purified by chromatography on silica using cyclohexane/ethyl acetate to give pure (R)-N-(bis(4-methoxyphenyl)(phenyl)methyl)-5-(5-bromo-2-fluorophenyl)-6,6-difluoro-5-methyl-2,5,6,7-tetrahydro-1,4-oxazepin-3-amine (A8A) as a colorless foam. MS (ISP): m/z=639.3 [M+H]+.

후처리

  1. washThe mixture was washed with saturated aqueous NH4Cl
  2. customthe organic layer was dried
  3. customevaporated
  4. customthe residue was purified by chromatography on silica

출처 및 근거

ORD 기록
ord-71adebc7ada1448ab9a67a14a2272af7
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08673894B2

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