Hydrochloric Acid → 3-Chloro-alpha-[[[1,1-dimethylethyl]amino]methyl]benzenemethanol hydrochloride salt

HRID 1090616노트

반응식

HRID 1090616 반응식
B.CSC.[CH3:5][C:6]([NH:9][C:10](=O)[CH:11]([OH:19])[C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([Cl:18])[CH:13]=1)([CH3:8])[CH3:7].CO.Cl>O1CCCC1>[ClH:18].[Cl:18][C:14]1[CH:13]=[C:12]([CH:11]([CH2:10][NH:9][C:6]([CH3:8])([CH3:7])[CH3:5])[OH:19])[CH:17]=[CH:16][CH:15]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 12423031(Dimethyl sulfide)trihydroboronHCID 19913633N-[1,1-dimethylethyl]-3-chloro-alpha-hydroxybenzeneacetamide

생성물 1

HCID 199136423-Chloro-alpha-[[[1,1-dimethylethyl]amino]methyl]benzenemethanol hydrochloride salt

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Borane-methyl sulphide (2.15g, 2.7ml, 4 equivs.) was added dropwise, under nitrogen, to a stirred solution of N-[1,1-dimethylethyl]-3-chloro-α-hydroxybenzene acetamide (1.71g) in dry tetrahydrofuran. The resulting solution was stirred and heated under reflux for 2h., cooled, and treated with methanol (1ml). The reaction mixture was heated under reflux for 1 h., cooled, treated with methanolic hydrogen chloride, and the solvent evaporated to give 3-chloro-α-[[[1,1-dimethylethyl]amino]methyl]benzenemethanol hydrochloride salt, 1.5g, m.p. 165-175° C.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 2h.
  3. temperaturecooled
  4. temperatureThe reaction mixture was heated
  5. temperatureunder reflux for 1 h.
  6. temperaturecooled
  7. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-6c71fadbafc24334ab2c0e4f5f6016bb
출처 데이터셋
uspto-grants-1992_01
특허 번호
US05082840

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