Dimethylformamide → HCID 90136031, 화합물

HRID 2275797노트

반응식

HRID 2275797 반응식
[NH2:1][CH2:2][CH:3]([OH:9])[CH2:4][O:5][CH:6]([CH3:8])[CH3:7].Cl[C:11]([O:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[O:12].C(N(C(C)C)CC)(C)C.CN(C=O)C>C1COCC1>[OH:9][CH:3]([CH2:4][O:5][CH:6]([CH3:8])[CH3:7])[CH2:2][NH:1][C:11](=[O:12])[O:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 10387Benzyl chloroformateHCID 81531DiisopropylethylamineHCID 6623501-Amino-3-isopropoxy-propan-2-ol

생성물 1

HCID 90136031HCID 90136031, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

1 g of rac-1-amino-3-isopropoxypropan-2-ol (7.5 mmol, 1 equivalent) were initially charged in 25 ml of THF, and 1.16 ml of benzyl chloroformate (8.3 mmol, 1.1 equivalents), 3.9 ml of diisopropylethylamine (22.5 mmol, 3 equivalents) and 183 mg of N,N-dimethylaminopyridine (1.5 mmol, 0.2 equivalents) were added. The reaction mixture was stirred at RT, and after about 30 min 5 ml of DMF were added. After a further 2.5 h at RT, the mixture was concentrated to dryness. The residue was taken up in ethyl acetate and washed with saturated aqueous sodium bicarbonate solution and then with saturated aqueous sodium chloride solution. The organic phase was dried over magnesium sulphate, filtered and concentrated. The residue was used without further purification for the next reaction.

후처리

  1. concentrationthe mixture was concentrated to dryness
  2. washwashed with saturated aqueous sodium bicarbonate solution
  3. dry with materialThe organic phase was dried over magnesium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was used without further purification for the next reaction

출처 및 근거

ORD 기록
ord-01e565fc6cd34823ab50ff6ba55b6e18
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09126998B2

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