Triethylamine → 7,8-Dimethoxy-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carbonyl chloride

HRID 657572노트

반응식

HRID 657572 반응식
O=C(Cl)[O:3][C:4]([Cl:7])(Cl)Cl.[CH3:9][O:10][C:11]1[C:21]([O:22][CH3:23])=[CH:20][C:14]2[CH2:15][CH2:16][NH:17][CH2:18][CH2:19][C:13]=2[CH:12]=1.C(N(CC)CC)C>ClCCl>[CH3:9][O:10][C:11]1[C:21]([O:22][CH3:23])=[CH:20][C:14]2[CH2:15][CH2:16][N:17]([C:4]([Cl:7])=[O:3])[CH2:18][CH2:19][C:13]=2[CH:12]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10426DiphosgeneHCID 129234297,8-Dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepine

생성물 1

HCID 866286287,8-Dimethoxy-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carbonyl chloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To 1.2 mL (10 mmol/1 eq.) of diphosgene in 20 mL of dichloromethane, at about 0° C., there are added, dropwise, a solution of 3.55 g (20 mmol) of 7,8-dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepine in 22 mL of dichloromethane, and then 4.2 mL (30 mmol/1.5 eq.) of triethylamine. Stirring overnight at ambient temperature and then concentration are carried out. The residue is taken up in dichloromethane, washed with water and dried over magnesium sulphate to yield, after concentration, the desired product.

후처리

  1. concentrationconcentration
  2. washwashed with water
  3. dry with materialdried over magnesium sulphate
  4. customto yield
  5. concentrationafter concentration

출처 및 근거

ORD 기록
ord-e3fb737e68f447fc86c7a2affe197dae
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08076325B2

반응 노트

불러오는 중…