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

HRID 1668563ノート

反応式

HRID 1668563 の反応式
[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

参加物

4

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f8680d12a6af41909e78f144fffb6e1f
出典データセット
uspto-grants-2011_08
特許番号
US07989444B2

反応ノート

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