Dichloromethane → Hydrochloric Acid

HRID 981671노트

반응식

HRID 981671 반응식
[CH3:1][O:2][C:3]1[C:8]2[CH2:9][CH:10]([NH2:13])[CH2:11][S:12][C:7]=2[CH:6]=[CH:5][CH:4]=1.[C:14](OC(=O)C)(=O)[CH3:15].C(Cl)[Cl:22]>>[ClH:22].[ClH:22].[CH2:14]([NH:13][CH:10]1[CH2:9][C:8]2[C:3]([O:2][CH3:1])=[CH:4][CH:5]=[CH:6][C:7]=2[S:12][CH2:11]1)[CH3:15]

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 7918Acetic AnhydrideHCID 143304585-Methoxy-3,4-dihydro-2H-1-benzothiopyran-3-amine

생성물 2

HCID 313Hydrochloric AcidHCID 14330486HCID 14330486, 화합물

실험 절차

A mixture of 500 mg of 3,4-dihydro-5-methoxy-2H-[1]-benzothiopyran-3-amine and 361 mg of acetic anhydride in 10 mL of methylene chloride is kept at room temperature of 15 min. The solvent is removed in vacuo and the resulting 3,4-dihydro-N-acetyl-5-methoxy-2H-[1]-benzopyran-3-amine is dissolved in 10 mL of 1M diborane in tetrahydrofuran. After 3 hr reflux, the reaction mixture is poured into 6N hydrochloric acid, washed with ether, basified with 45% potassium hydroxide and reextracted with ether. After drying over magnesium sulfate, the solvent is removed in vacuo. Acidification with ethanolic hydrochloric acid affords 3,4-dihydro-N-ethyl-5-methoxy-2H-[1]-benzothio-pyran-3-amine hydrochloride melting at 222°-224°.

후처리

  1. customThe solvent is removed in vacuo
  2. dissolutionthe resulting 3,4-dihydro-N-acetyl-5-methoxy-2H-[1]-benzopyran-3-amine is dissolved in 10 mL of 1M diborane in tetrahydrofuran
  3. temperatureAfter 3 hr reflux
  4. additionthe reaction mixture is poured into 6N hydrochloric acid
  5. washwashed with ether
  6. dry with materialAfter drying over magnesium sulfate
  7. customthe solvent is removed in vacuo

출처 및 근거

ORD 기록
ord-8d79b46093c8497a844a1e14a40bd1b2
출처 데이터셋
uspto-grants-1991_02
특허 번호
US04992465

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