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4-Methylmorpholine → isobutyl N-[9-(3,17beta-dihydroxyoestra-1,3,5(10)-trien-7alpha-yl)nonyl]-N-methylcarbamoate

HRID 543018
ノート
印刷プレビュー

反応式

HRID 543018 の反応式
CN1CCOCC1.Cl[C:9]([O:11][CH2:12][CH:13]([CH3:15])[CH3:14])=[O:10].[CH3:16][NH:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][C@@H:27]1[CH2:44][C:43]2[CH:42]=[C:41]([OH:45])[CH:40]=[CH:39][C:38]=2[C@@H:37]2[C@@H:28]1[C@H:29]1[C@@:33]([CH2:35][CH2:36]2)([CH3:34])[C@@H:32]([OH:46])[CH2:31][CH2:30]1.C(=O)(O)[O-].[Na+]>O1CCCC1>[OH:45][C:41]1[CH:40]=[CH:39][C:38]2[C@@H:37]3[C@H:28]([C@H:29]4[C@@:33]([CH2:35][CH2:36]3)([CH3:34])[C@@H:32]([OH:46])[CH2:31][CH2:30]4)[C@H:27]([CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][N:17]([CH3:16])[C:9](=[O:10])[O:11][CH2:12][CH:13]([CH3:15])[CH3:14])[CH2:44][C:43]=2[CH:42]=1
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 79724-MethylmorpholineHCID 62365Isobutyl chloroformateHCID 516892Sodium BicarbonateHCID 543355367alpha-(9-Methylaminononyl)oestra-1,3,5(10)-triene-3,17beta-diol

生成物 1

HCID 70447132isobutyl N-[9-(3,17beta-dihydroxyoestra-1,3,5(10)-trien-7alpha-yl)nonyl]-N-methylcarbamoate

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

N-Methylmorpholine (0.028 ml.) and isobutyl chloroformate (0.038 ml.) were successively added to a stirred solution of 7α-(9-methylaminononyl)oestra-1,3,5(10)-trien-3,17β-diol (Example 28; 0.08 g.) in tetrahydrofuran (3 ml.) and the mixture was stirred at laboratory temperature for 150 minutes. Saturated aqueous sodium bicarbonate solution (2 ml.) was added and the mixture was extracted three times with methylene chloride (10 ml. each time). The combined extracts were washed with water (5 ml.), dried and evaporated to dryness and there was thus obtained as residual oil isobutyl N-[9-(3,17β-dihydroxyoestra-1,3,5(10)-trien-7α-yl)nonyl]-N-methylcarbamoate.

後処理

  1. extractionthe mixture was extracted three times with methylene chloride (10 ml
  2. washThe combined extracts were washed with water (5 ml.)
  3. customdried
  4. customevaporated to dryness and there

出典と根拠

ORDレコード
ord-3b9b5f4e451c4dc8a22c6f2d88fc1100
出典データセット
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04659516

反応ノート

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