Hydrochloric Acid → HCID 70578051, 화합물

HRID 225305

반응식

HRID 225305 반응식
[NH2:1][CH:2]([C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1)[C:3]([OH:5])=[O:4].[ClH:13].[CH2:14]=O>CO>[ClH:13].[NH2:1][CH:2]([C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[C:8]([CH2:14][Cl:13])[CH:7]=1)[C:3]([OH:5])=[O:4]

참가 물질

5

반응물 3

HCID 313Hydrochloric Acid2회HCID 712FormaldehydeHCID 921434-Hydroxyphenylglycine

생성물 1

HCID 70578051HCID 70578051, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of (-)-α-amino-4-hydroxybenzeneacetic acid (100 g, 0.6 mole) in a minimum amount of concentrated hydrochloric acid at 35°-40° C. is added 50 ml of aqueous formaldehyde (35-37%) (0.6 mole). The addition of hydrogen chloride gas is begun. After 5-10 minutes, a solid begins to precipitate. Stirring is continued for 30 minutes, and the solid is then collected. The crude product is washed with ether and with acetone. A second crop is obtained from the filtrate after standing at room temperature overnight. Total yield is 102 g (67%) m.p. >300° C., [α]D18 =-134° (c 4.75, CH3OH) NMR (DMSO-D6) ppm (δ) 4.68 (s,2), 4.9 (broad s,1), 6.9-7.6 (superimposed q and s,3).

후처리

  1. customto precipitate
  2. waitis continued for 30 minutes
  3. customthe solid is then collected
  4. washThe crude product is washed with ether and with acetone
  5. customA second crop is obtained from the filtrate
  6. waitafter standing at room temperature overnight

출처 및 근거

ORD 기록
ord-5af12cd787af44039489c0a8ab470093
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04236002

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