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Stearoyl chloride → HCID 20249612、化合物

HRID 1077116
ノート
印刷プレビュー

反応式

HRID 1077116 の反応式
[OH:1][CH2:2][C:3]12[CH2:10][O:9][P:6]([O:7][CH2:8]1)[O:5][CH2:4]2.[C:11](Cl)(=[O:29])[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28].C(N(CC)CC)C>C1(C)C=CC=CC=1>[P:6]12[O:9][CH2:10][C:3]([CH2:2][O:1][C:11](=[O:29])[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])([CH2:8][O:7]1)[CH2:4][O:5]2
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8212Stearoyl chlorideHCID 8471TriethylamineHCID 200183Pentaerythritol phosphite

生成物 1

HCID 20249612HCID 20249612、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

16.4 g (0.1 mol) of 4-hydroxymethyl-1-phospha-2,6,7-trioxabicyclo[2,2,2]octane are dissolved in 150 ml of toluene by warming. 30.2 g (0.1 mol) of stearic acid chloride, followed by 10.1 g (0.1 mol) of triethylamine, are added dropwise at room temperature. After the slight evolution of heat has died away, the mixture is stirred for 10 hours under nitrogen at room temperature and the precipitated triethylamine hydrochloride is then filtered off. The filtrate is evaporated with exclusion of moisture, a yellowish oil remaining, which crystallises on being triturated with methanol. After filtering off under suction and drying, stearic acid 1-phospha-2,6,7-trioxabicyclo[2,2,2]oct-4-yl-methyl ester (Stabiliser No. 9), melting point 49°C, is obtained.

後処理

  1. temperatureby warming
  2. additionare added dropwise at room temperature
  3. temperatureAfter the slight evolution of heat
  4. filtrationthe precipitated triethylamine hydrochloride is then filtered off
  5. customThe filtrate is evaporated with exclusion of moisture
  6. customwhich crystallises
  7. customon being triturated with methanol
  8. filtrationAfter filtering off under suction
  9. customdrying

出典と根拠

ORDレコード
ord-c2a9fb2568c74e0e9c13a88c9bb1392a
出典データセット
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03959413

反応ノート

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