Methanol → HCID 22591851, 화합물

HRID 749512노트

반응식

HRID 749512 반응식
[NH2:1][CH:2]([C:7]1[CH:16]=[CH:15][C:10]2[O:11][CH2:12][CH2:13][O:14][C:9]=2[CH:8]=1)[CH2:3][C:4]([OH:6])=[O:5].S(Cl)(Cl)=O.[CH3:21]O>>[NH2:1][CH:2]([C:7]1[CH:16]=[CH:15][C:10]2[O:11][CH2:12][CH2:13][O:14][C:9]=2[CH:8]=1)[CH2:3][C:4]([O:6][CH3:21])=[O:5]

참가 물질

4

반응물 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 35364503-amino-3-(2,3-dihydro-1,4-benzodioxin-6-yl)propanoic acid

생성물 1

HCID 22591851HCID 22591851, 화합물

실험 절차

3-Amino-3-(2,3-dihydro-1,4-benzodioxin-6-yl)propionic acid [synthesis according to instructions known from the literature (e.g., L. Lázár, T. Martinek, G. Bernáth, F. Fülöp, Synth. Comm. 1998, 28, 219-224)]is introduced into a vessel in methanol (about 0.5 to 1.0 mol/l) and admixed dropwise at 0° C. with 1.2 eq of thionyl chloride. When the addition has been made the reaction mixture is stirred at room temperature overnight and subsequently concentrated. The residue is dissolved in a little methanol and the product is precipitated with diethyl ether. The solid is filtered off with suction, washed repeatedly with diethyl ether and dried under reduced pressure.

후처리

  1. additionWhen the addition
  2. concentrationsubsequently concentrated
  3. dissolutionThe residue is dissolved in a little methanol
  4. customthe product is precipitated with diethyl ether
  5. filtrationThe solid is filtered off with suction
  6. washwashed repeatedly with diethyl ether
  7. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-574582ea62f643f28a2b4325e5801890
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07402683B2

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