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Hydrazine hydrate (1:1) → 12-Amino-1-dodecanol

HRID 1003308
ノート
印刷プレビュー

反応式

HRID 1003308 の反応式
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][N:14]1C(=O)C2=CC=CC=C2C1=O.O.NN>CO>[NH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][OH:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 18796407N-(12-hydroxydodecyl)phthalimide

生成物 1

HCID 518202012-Amino-1-dodecanol収率 74.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In 600 ml of methanol was dissolved while warming 48.0 g of N-(12-hydroxydodecyl)phthalimide, 50 ml of hydrazine monohydrate was added at room temperature with stirring and the mixture was stirred overnight. The crystal thus separated out was filtered off and the solvent was distilled off. The residue was extracted with hot chloroform and insolubles were filtered off. The filtrate was distilled, the residue was extracted with hot chloroform (100 ml×3) and then the solvent was distilled off. The residue was dissolved in methanol and recrystallization from methanol-ethyl acetate gave 21.6 g of the title compound as a crystal.

後処理

  1. additionwas added at room temperature
  2. stirringthe mixture was stirred overnight
  3. customThe crystal thus separated out
  4. filtrationwas filtered off
  5. distillationthe solvent was distilled off
  6. extractionThe residue was extracted with hot chloroform and insolubles
  7. filtrationwere filtered off
  8. distillationThe filtrate was distilled
  9. extractionthe residue was extracted with hot chloroform (100 ml×3)
  10. distillationthe solvent was distilled off
  11. dissolutionThe residue was dissolved in methanol
  12. customrecrystallization from methanol-ethyl acetate

出典と根拠

ORDレコード
ord-c7baf5ca20614e9b99493d1848dede8b
出典データセット
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06046201

反応ノート

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