Triethylamine → 1-(Diphenylmethyl)-2-azetidinecarboxaldehyde

HRID 1702759노트

반응식

HRID 1702759 반응식
Cl.[CH:2]([N:15]1[CH2:18][CH2:17][CH:16]1[CH2:19][OH:20])([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(N(CC)CC)C>CS(C)=O>[CH:2]([N:15]1[CH2:18][CH2:17][CH:16]1[CH:19]=[O:20])([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1

참가 물질

4

반응물 2

HCID 8471TriethylamineHCID 12717144[1-(Diphenylmethyl)azetidin-2-yl]methanol--hydrogen chloride (1/1)

생성물 1

HCID 127171451-(Diphenylmethyl)-2-azetidinecarboxaldehyde

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매2회

실험 절차

To a stirred mixture of 9.0 g of 1-benzhydrylazetidine-2-methanol hydrochloride, 26.1 ml of triethylamine and 60 ml of dimethylsulfoxide were added dropwise a solution of 14.9 g pyridine-sulfur trioxide complex in 60 ml of dimethylsulfoxide. The mixture was stirred at room temperature for 30 minutes, after which it was poured into ice water and extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate, followed by removal of the solvent by distillation. The residue was recrystallized from n-hexane to yield 1-benzhydrylazetidine-2-carbaldehyde as colorless crystals melting at 88°-89° C.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customfollowed by removal of the solvent by distillation
  5. customThe residue was recrystallized from n-hexane

출처 및 근거

ORD 기록
ord-ae2f7d52bed944d19da01b4b64129f77
출처 데이터셋
uspto-grants-1982_09
특허 번호
US04349547

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