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Water → 3beta-Caprylamido-7alpha,12alpha-dihydroxy-5beta-cholan-24-oic methylester

HRID 1934326
ノート
印刷プレビュー

反応式

HRID 1934326 の反応式
[CH3:1][O:2][C:3](=[O:30])[CH2:4][CH2:5][C@H:6]([C@@H:8]1[C@:25]2([CH3:26])[C@H:11]([C@H:12]3[C@H:22]([CH2:23][C@@H:24]2[OH:27])[C@:20]2([CH3:21])[C@@H:15]([CH2:16][C@@H:17]([NH2:28])[CH2:18][CH2:19]2)[CH2:14][C@H:13]3[OH:29])[CH2:10][CH2:9]1)[CH3:7].C(N([CH2:36][CH3:37])CC)C.[C:38](Cl)(=[O:44])[CH2:39][CH2:40][CH2:41][CH2:42][CH3:43].O>C(Cl)Cl>[CH3:1][O:2][C:3](=[O:30])[CH2:4][CH2:5][C@H:6]([C@@H:8]1[C@:25]2([CH3:26])[C@H:11]([C@H:12]3[C@H:22]([CH2:23][C@@H:24]2[OH:27])[C@:20]2([CH3:21])[C@@H:15]([CH2:16][C@@H:17]([NH:28][C:38](=[O:44])[CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:36][CH3:37])[CH2:18][CH2:19]2)[CH2:14][C@H:13]3[OH:29])[CH2:10][CH2:9]1)[CH3:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 67340Hexanoyl chlorideHCID 10364902HCID 10364902、化合物

生成物 1

HCID 865854493beta-Caprylamido-7alpha,12alpha-dihydroxy-5beta-cholan-24-oic methylester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane
溶媒
2 回

実験手順

1.0 g of 3β-amino-7α,12α-dihydroxy-5β-cholan-24-oic methylester (FIG. 5A-1) [see Example I] were dissolved in 30 ml dry methylene chloride and treated with 15 ml triethyl amine under stirring. 1.2 g of caproyl chloride acid in 10 ml methylene chloride were added dropwise to the resulting solution, and the stirring was continued overnight. The reaction mixture was poured into water extracted with methylene chloride, the organic fraction was then dried over sodium sulfate, evaporated to dryness and chromatographed over silica gel with a mixture of ethyl acetate and hexane (6:4 and 8:2), to give 0.7 g 3β-caprylamido-7α,12α-dihydroxy-5β-cholan-24-oic methylester (FIG. 5A-14).

後処理

  1. extractionextracted with methylene chloride
  2. dry with materialthe organic fraction was then dried over sodium sulfate
  3. customevaporated to dryness
  4. customchromatographed over silica gel with a mixture of ethyl acetate and hexane (6:4 and 8:2)

出典と根拠

ORDレコード
ord-a66d04a977e94e50b0d82ab2c56e7107
出典データセット
uspto-grants-2002_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06384024B1

反応ノート

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