Ethanol → Phosphoric acid--benzyl 5-amino-4-oxopentanoate (1/1)

HRID 222818ノート

反応式

HRID 222818 の反応式
Cl.[CH2:2]([O:9][C:10](=[O:17])[CH2:11][CH2:12][C:13]([CH2:15][NH2:16])=[O:14])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[P:18](=[O:22])([OH:21])([OH:20])[OH:19].C(N(CC)CC)C.C(O)C>O>[P:18]([OH:22])([OH:21])([OH:20])=[O:19].[CH2:2]([O:9][C:10](=[O:17])[CH2:11][CH2:12][C:13]([CH2:15][NH2:16])=[O:14])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

参加物

6

反応物 4

HCID 702EthanolHCID 1004Phosphoric AcidHCID 8471TriethylamineHCID 22253144Benzyl 5-amino-4-oxopentanoate--hydrogen chloride (1/1)

生成物 1

HCID 66932752Phosphoric acid--benzyl 5-amino-4-oxopentanoate (1/1)

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A 8 g (31 mmol) portion of δ-aminolevulinic acid benzyl ester hydrochloride and 4 g (34.7 mmol) of 85% phosphoric acid were dissolved in 8 ml of purified water, and 3.3 g (32.7 mmol) of triethylamine was added dropwise thereto while stirring on an ice bath. After completion of the dropwise addition and subsequent stirring at room temperature for 10 minutes, 300 ml of ethanol was added thereto and stirred. The thus precipitated precipitate was recovered by suction filtration and dried at room temperature for 16 hours under a reduced pressure. An 8.5 g (27 mmol) portion of δ-aminolevulinic acid benzyl ester phosphate was obtained at a yield of 87 mol %.

後処理

  1. additionAfter completion of the dropwise addition
  2. stirringsubsequent stirring at room temperature for 10 minutes
  3. stirringstirred
  4. filtrationThe thus precipitated precipitate was recovered by suction filtration
  5. customdried at room temperature for 16 hours under a reduced pressure

出典と根拠

ORDレコード
ord-a356a005f0574bdca6fd9cd64faec519
出典データセット
uspto-grants-2012_06
特許番号
US08207376B2

反応ノート

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