Hydrochloric Acid → HCID 70578051、化合物

HRID 225305

反応式

HRID 225305 の反応式
[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]

参加物

5

反応物 3

HCID 313Hydrochloric Acid2 回HCID 712FormaldehydeHCID 921434-Hydroxyphenylglycine

生成物 1

HCID 70578051HCID 70578051、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-5af12cd787af44039489c0a8ab470093
出典データセット
uspto-grants-1980_11
特許番号
US04236002

関連ノート

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