Hydrochloric Acid → 5-Amino-7-chloro-9-methyl-2,3,4,5-tetrahydro-1-benzoxepine

HRID 2271081노트

반응식

HRID 2271081 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH3:14])[C:5]2[O:11][CH2:10][CH2:9][CH2:8][C:7](=O)[C:6]=2[CH:13]=1.C([O-])(=O)C.[NH4+].C([BH3-])#[N:21].[Na+].Cl>CO>[NH2:21][CH:7]1[C:6]2[CH:13]=[C:2]([Cl:1])[CH:3]=[C:4]([CH3:14])[C:5]=2[O:11][CH2:10][CH2:9][CH2:8]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 517165Ammonium AcetateHCID 43472547-Chloro-9-methyl-3,4-dihydro-2H-benzo[b]oxepin-5-oneHCID 5003444Sodium cyanoborohydride

생성물 1

HCID 223917895-Amino-7-chloro-9-methyl-2,3,4,5-tetrahydro-1-benzoxepine수율 61.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

3.0 g of 7-chloro-9-methyl-3,4-dihydro-2H-1-benzoxepin-5-one, 50 ml of anhydrous methanol, 10.9 g of ammonium acetate and 0.63 g of sodium cyanoborohydride were stirred for 5 h at 60° C. and then for 2 days at RT. The reaction mixture was then acidified with hydrochloric acid and then concentrated on a rotary evaporator. The residue was taken up in water, and the solution was rendered alkaline with ammonia solution and extracted with EA. After drying and concentrating, the product was purified by chromatography on silica gel using ethyl acetate/methanol 9:1 and 1.3 g of 5-amino-7-chloro-9-methyl-2,3,4,5-tetrahydro-1-benzoxepine were obtained.

후처리

  1. concentrationconcentrated on a rotary evaporator
  2. extractionextracted with EA
  3. customAfter drying
  4. concentrationconcentrating
  5. customthe product was purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-f5c39af47cb646ce8e7c41d37c4c9f3d
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06333349B1

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