Trifluoroacetic acid → 2-Methyl-6,7,8,9-tetrahydro-5H-[1,3]oxazolo[4,5-h][3]benzazepine

HRID 1668563노트

반응식

HRID 1668563 반응식
[CH3:1][C:2]1[O:3][C:4]2[C:21]([N:22]=1)=[CH:20][C:7]1[CH2:8][CH2:9][N:10](C(OC(C)(C)C)=O)[CH2:11][CH2:12][C:6]=1[CH:5]=2.FC(F)(F)C(O)=O>C(Cl)Cl>[CH3:1][C:2]1[O:3][C:4]2[C:21]([N:22]=1)=[CH:20][C:7]1[CH2:8][CH2:9][NH:10][CH2:11][CH2:12][C:6]=1[CH:5]=2

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 591504881,1-Dimethylethyl 2-methyl-5,6,8,9-tetrahydro-7H-[1,3]oxazolo[4,5-h][3]benzazepine-7-carboxylate

생성물 1

HCID 591504802-Methyl-6,7,8,9-tetrahydro-5H-[1,3]oxazolo[4,5-h][3]benzazepine수율 114.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1,1-Dimethylethyl 2-methyl-5,6,8,9-tetrahydro-7H-[1,3]oxazolo[4,5-h][3]benzazepine-7-carboxylate (1.1 g) was exposed to trifluoroacetic acid (5 ml) in DCM (5 ml) for 90 min at 25° C. After elimination of volatiles under reduced pressure the residue was partitioned between aqueous Na2CO3 (2M) and DCM. The organic layer was collected and the aqueous phase extracted twice with DCM. The combined DCM layers were concentrated to give the title compound (0.84 g) as an off-white solid.

후처리

  1. customAfter elimination of volatiles under reduced pressure the residue was partitioned between aqueous Na2CO3 (2M) and DCM
  2. customThe organic layer was collected
  3. extractionthe aqueous phase extracted twice with DCM
  4. concentrationThe combined DCM layers were concentrated

출처 및 근거

ORD 기록
ord-f8680d12a6af41909e78f144fffb6e1f
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07989444B2

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